CN101717905A - Method and device for preparing high-performance aluminum-base composite material under the action of pulsed magnetic field - Google Patents
Method and device for preparing high-performance aluminum-base composite material under the action of pulsed magnetic field Download PDFInfo
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Abstract
The invention provides a method and a device for preparing high-performance aluminum-base composite material under the action of the pulsed magnetic field with the in situ crystallization method, belonging to the technical field of material preparation. The method comprises the following steps: smelting to synthesize compound material melt at the temperature of 10-200 DEG C higher than the compound material melt liquidus temperature and pouring the compound material melt into a specially-designed crystallizer to make the compound material melt solidify under the action of the pulsed magnetic field. The pulsed magnetic field has the key parameters of the pulse width of 1-500 ms and the amplitude strength of 0.1-50T. The pulsed electromagnetic force is applied to the process of solidifying the compound material melt under the action of the pulsed magnetic field so as to refine the matrix structure and the particle reinforced phase of the compound material at the same time, control the growth of the particle reinforced phase in cluster, increase the bonding strength of the interface of the particle reinforced phase and the matrix and obviously improve the performance of the composite material.
Description
Technical field
The present invention relates to the Composite Preparation technical field, specially refer to and utilize in-situ crystallization technique to prepare the method and apparatus of high-performance in-situ authigenic aluminum matrix composite under a kind of pulsed magnetic field action.
Background technology
Particle enhanced aluminum-based composite material becomes a kind of application type material more and more widely gradually because of having compound constitutional features and good physics and chemistry and mechanical property.At present, in-situ compositing is the important method of preparation particle enhanced aluminum-based composite material.Because wild phase original position forming core from aluminum substrate of in-situ compositing is separated out, has higher thermodynamic stability, and compound and matrix bond interface cleanliness factor height, wettability is good, and the bonding strength height is when guaranteeing that material has preferably toughness and high-temperature behavior, the intensity and the Young's modulus of material have been improved greatly, so in-situ compositing is that the preparation high performance composite have performance advantage, enjoys attention.
In-situ compositing can be divided into reaction in composite algorithm and in-situ crystallization composite algorithm again according to the generating mode difference that strengthens body.Reaction in is compound to be by adding reactant in melt, forming tiny stable enhanced granule method mutually by the reactant and the in-situ chemical reaction of matrix metal; The in-situ crystallization compound rule is the phase transformation that utilizes in binary or the multicomponent alloy process of setting, separates out enhancing body particle and prepare aluminum matrix composite from alloy liquid.The major advantage of in-situ crystallization composite algorithm is can cross means such as cold by control solidification and crystallization time and Tc and bath composition to control and separate out particle kind, quantity mutually, so the in-situ crystallization process is easier to control.
Along with expanding economy, human requirement to the raising material property is endless.At present, the key factor that restriction particle enhanced aluminum-based composite material performance further improves has two aspects: the one, and the tissue of metallic matrix, performance and need to improve with particle coupling mutually, its key is to want the grain structure of refinement matrix, the performance of raising matrix; The 2nd, the size of enhanced granule phase wants further refinement, particle phase pattern more regular, its distribution in matrix will be more even and the bonding interface intensity of particle and matrix need further raising.
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, carry out with the promotion reaction in, but the process of setting of melt is not controlled.Chinese patent CN101391290A proposes the method for the synthetic metal-base composites of fusant reaction under a kind of magnetic field and the ultrasonic field coupling, does not also mention the process of setting of melt is controlled.Chinese patent: CN 101199989, the alien frequencies composite electromagnetic is the method for continuous casting particulate reinforced metal matrix matrix material after the match, proposition applies alien frequencies (low frequency, high frequency) resultant field at process of setting, low frequency magnetic field is used to overcome the particulate cluster, high frequency magnetic field is used to improve cc billet surface quality, but because enhanced granule is that step of reaction forms and grows up in position, low frequency magnetic field makes the endocorpuscular thinning effect of melt not obvious.Above prior art all is to prepare matrix material at the method that generates enhanced granule by reaction in, the particle that this reaction in generates generates in the compounding flux building-up process, cluster is grown up easily in follow-up coagulation forming process, and the wild phase granule strength of growing up is very high, is difficult to its refinement.
Chinese patent CN100345224C proposes in-situ authigenic MgB under the pulsed magnetic field action
2The preparation method of superconducting material, this invention is to adopt powder metallurgy method, can control matrix and prevent that particle clusters is with poly-partially, but this preparation method needs abrasive dust, pressing mold to encapsulate, vacuumize, fill processes such as nitrogen, complicated process of preparation, cost is higher, and most important deficiency is the most important link of powder metallurgic method preparation technique---and the different factor of sample inside and outside temperature difference is difficult to overcome in the sintering process, so powder metallurgy process also is difficult to prepare large-sized blank to produce large-sized structural parts.Metal melt synthetic composite material and the method by casting prepare matrix material and are suitable for industrial-scale production, and technological process is simple relatively, and manufacturing cost is cheap relatively.But lack at present Composite Melt casting process of setting refinement matrix solidified structure and control particle mutually cluster grow up and gather uneven effective ways partially.Chinese patent CN1261612C (denomination of invention: high-intensity magnetic field prepares the method and the device of aluminum matrix composite down) proposes to apply high-intensity magnetic field in aluminum matrix composite melt solidifying process, improve the preferred orientation coefficient of enhanced granule distribution consistency degree and enhancing staple fibre, thereby improve composite material combination property.Though should invent the high-intensity magnetic field of also undeclared its use is the high-intensity magnetic field of which kind of form, but utilize " little (surpassing) gravitational effects (being magnetic levitation), crystal preferred orientation effect and convection current suppress effect " in magnetic field to judge that its high-intensity magnetic field that uses is steady strong magnetic field from this invention.The Composite Melt process of setting applies steady strong magnetic field, and the preferred orientation effect that strengthens whisker or staple fibre is obvious, but steady strong magnetic field is difficult to make the grain refining of enhanced granule phase and matrix.
In sum, reaction in is generated the particle legal system to be equipped with matrix material and to adopt particle to add legal system and be equipped with matrix material, because particle is at compounding flux preparation process forming core or grow up, cluster in process of setting, also can occur and grow up, so the present invention adopts in-situ crystallization technique to prepare matrix material, and propose at the melt solidifying crystallisation process, it also is enhanced granule forming core precipitation process, apply pulsed magnetic field, can promote crystallization nucleation, make the effective refinement of grain structure and increase the instantaneous nucleation rate of in-situ crystallization particle simultaneously, make the particle wild phase and the refinement simultaneously of matrix metal crystal grain of matrix material, and control particle phase cluster and grow up and poly-partially uneven method, significant to the performance that improves particle enhanced aluminum-based composite material.
Summary of the invention
The purpose of this invention is to provide and utilize in-situ crystallization technique to prepare the method and apparatus of high-performance particle enhanced aluminum-based composite material under a kind of pulsed magnetic field action, promptly the solidification and crystallization process by using at compounding flux applies pulsed magnetic field, the pulse-electromagnetic force effect that utilizes pulsed magnetic field and the solidified structure of pulse induction thermal shocking effect refinement aluminum substrate and the cluster of simultaneously the in-situ crystallization particle being carried out refinement, control particle phase are mutually grown up, and overcome the poly-partially uneven distribution problem of particle, with preparation very-high performance particulate reinforced composite.
The objective of the invention is to realize by following technical proposal:
The first step: the preparation of Composite Melt
The melt preparation that in-situ crystallization technique prepares matrix material mainly is an alloying process, earlier aluminum or aluminum alloy is melted, the composition of determining alloy melt according to the wild phase volume fraction of wild phase kind and requirement carries out alloying, the alloying temperature is determined according to element solubleness and alloy melting temperature, the alloying temperature is higher 10～200 ℃ than alloy melt liquidus temperature, strengthens body and can select Si phase, Al
3Ti or Mg
2Si.
The compounding flux preparation process is opened induction stirring magnetic field 1 and is carried out induction stirring, the frequency-tuning range in induction stirring magnetic field is 1～30Hz, the strength of current regulation range is: 100～750A, by control current intensity and power frequency, make melt that suitable stirring intensity be arranged, can promote composition, temperature even, not destroy weld pool surface insulating covering agent or oxidation film layer again.
Second step: Composite Melt is solidified under pulsed magnetic field action
The present invention adopts the conventional pulsed magnetic field generating unit that uses, and uses key parameter to be pulsewidth 1～500ms, the pulsed magnetic field amplitude intensity 0.1～50T of generation.Crystallizer adopts to solidify under the custom-designed pulsed magnetic field uses crystallizer, crystallizer is divided into three sections from top to bottom by material: epimere is a refractory, major function is slow cooling, and the stage casing is a graphite annulus, promptly guarantees cooling, guarantee the indeformable and certain intensity of crystallizer again, hypomere is the water-cooled red copper, guarantees coldly by force, and the height ratio between three sections is 1: 2: 1, the pulsed magnetic field coil is installed on crystallizer graphite section, and hub of a spool and graphite section center are at sustained height.
Adopt operating process of the present invention to be characterized as: in the melting synthesis reactor, to prepare Composite Melt, the melting building-up process is opened induction stirring magnetic field and is stirred, promote that the composition temperature is even, after compounding flux prepares, open control stream stopper (or chute baffle plate), compounding flux is in cast in the heat top in water filling port (or chute) injection down, after liquid level rises to certain altitude, start the stripping device, simultaneously, the unbalanced pulse magnetic field device, compounding flux solidifies in special crystallizer under pulsed magnetic field action, by the position of control stripping speed and control stream stopper (or chute baffle plate), promptly keep the liquid level stabilizing in the casting heat top, the security deposit owner will be solidified in the pulsed magnetic field action scope again.
Compared with prior art the present invention has the following advantages and effect:
1) in-situ crystallization technique prepares particle enhanced aluminum-based composite material, crystallisation process applies pulsed magnetic field in position, the pulse-electromagnetic force impact effect of utilizing pulsed magnetic field and pulse induction thermal shocking effect change particle mutually the in-situ crystallization process and the process of setting of matrix metal, pulsed magnetic field has increased the fluctuation of energy of particle, the forming core speed and the nucleation rate of in-situ junction crystalline phase are improved, and can smash big particle by pulse action, make grain refine;
2) matrix metal is solidified, pulsed magnetic field impels solidified front and interdendritic crystallization rain backflow hunting speed to increase, refinement the nucleus size, increased the nucleus number, impel the solidified structure refinement of matrix;
3) oscillation action of the pulse-electromagnetic force of process of setting help particle mutually with matrix grain between coupling and interface combine, wettability is good, has improved particle mutually and high base strength.
Therefore, pulsed magnetic field action is in the in-situ crystallization process, realized simultaneously the refinement of matrix and original position wild phase and the dispersion of in-situ crystallization particle wild phase, and improved the interface bond strength of particle, effectively improved the over-all properties of particulate reinforced composite with matrix.
Description of drawings:
In-situ crystallization technique prepares high-performance aluminum-base composite material device synoptic diagram under Fig. 1 pulsed magnetic field
Caption: 1 induction stirring magnetic field; 2 heating systems; 3 melting synthesis reactor; 4 control stream stoppers (or chute baffle plate); 5 compounding flux; 6 times water filling ports (or chute); 7 thermometrics and temperature controlling system; 8 casting are pushed up with heat; 9 special crystallizers pottery section; 10 special crystallizer graphite annulus sections; 11 special crystallizer fine copper sections; 12 bed dies and stripping device; 13 semi-solid state strands (ingot); 14 pulsed magnetic field apparatus; 15 level monitorings and control;
Fig. 2 is solidified structure and the XRD detected result that applies pulsed magnetic field front and back in-situ crystallization Si particle enhanced aluminum-based composite material.(a) do not adopt the present invention; (b) adopt the present invention; (c) XRD detected result.
Fig. 3 applies pulsed magnetic field front and back in-situ crystallization Al
3The solidified structure and the XRD detected result of Ti particle reinforced aluminium-based (A356) matrix material.(a) do not adopt the present invention; (b) adopt the present invention; (c) XRD detected result.
Fig. 4 applies pulsed magnetic field front and back 20%Mg
2The solidified structure of Si particle enhanced aluminum-based composite material and XRD detected result.(a) do not adopt the present invention; (b) adopt the present invention; (c) XRD detected result.
Fig. 5 applies pulsed magnetic field front and back 10%Mg
2The solidified structure of Si particle enhanced aluminum-based composite material and XRD detected result.(a) do not adopt the present invention; (b) adopt the present invention; (c) EDS detected result.
Fig. 6 has contrasted and adopted embodiments of the invention 2 is the Al that obtains with not adopting the present invention
3The matrix grain size comparing result of Ti particle reinforced aluminium-based (A356) matrix material.(a) do not adopt the present invention; (b) adopt the present invention.
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.
In-situ crystallization prepares the primary silicon reinforced aluminum matrix composites under embodiment 1 pulsed magnetic field
Prepare silumin Al-18%Si with fine aluminium and silicon metal, 850 ℃ of synthesis temperatures, the parameter in preparation process induction stirring magnetic field is 15Hz, electric current 250A.The pulsewidth of process of setting pulsed magnetic field is 10ms, and pulsed magnetic field intensity is 30T, and stripping speed is 15cm/min, makes primary silicon enhanced aluminum matrix composite.
Fig. 2 is solidified structure and the XRD detected result that applies pulsed magnetic field front and back Si particle enhanced aluminum-based composite material.As seen from Figure 2: (1) by XRD as seen, in the solidified structure type of phase be α (Al) with Si mutually; (2) under the alloying constituent same case, apply behind the pulsed magnetic field Si particle and generate quantity and increase, particle size is reduced to 10～20 μ m by 50～60 μ m, and thinning effect is obvious, and particle size is even, and the homogenizing degree that distributes in matrix improves; (3) α (Al) is mutually fined, and promptly the matrix metal grain-size reduces, and the average grain size when not applying pulsed magnetic field is at 100～120 mu m ranges, apply pulsed magnetic field after average grain size refine to 30～50 μ m.Comprehensively it seems: apply in the process of setting that the solidified structure of matrix material is able to obvious improvement behind the pulsed magnetic field.
In-situ crystallization technique prepares Al under embodiment 2 pulsed magnetic fields
3Ti particle reinforced aluminium-based (A356) matrix material
The synthetic aluminum titanium alloy melt Al-5%Ti under 840 ℃ with A356 aluminium alloy and aluminum-titanium alloy, building-up process induction stirring magnetic field parameter is 1Hz, electric current 350A.The pulsewidth of process of setting pulsed magnetic field is 500ms, and pulsed magnetic field intensity is 10T, and stripping speed is 10cm/min, makes Al
3The Ti particle reinforced A 356 matrix composite material.
Fig. 3 applies pulsed magnetic field front and back Al
3The solidified structure of Ti particle enhanced aluminum-based composite material and XRD detected result.As seen from the figure: (1) is α (Al) and Al by the type that XRD figure draws phase in the solidified structure
3The Ti phase; (2) under the alloying constituent same case, apply behind the pulsed magnetic field Si particle and generate quantity and increase, particle size is reduced to 2～5 μ m by 10～20 μ m, and thinning effect is obvious, and the particle size degree of uniformity improves, and the homogenizing degree that distributes in matrix improves; (3) α (Al) is mutually fined, and promptly the matrix metal grain-size reduces, and the average grain size when not applying pulsed magnetic field is at 80～110 mu m ranges, apply pulsed magnetic field after average grain size refine to 10～20 μ m (comparing result is seen Fig. 6).Comprehensively it seems: apply in the process of setting that the solidified structure of matrix material is able to obvious improvement behind the pulsed magnetic field.
In-situ crystallization technique prepares 20%Mg under embodiment 3 pulsed magnetic fields
2The Si particle enhanced aluminum-based composite material
Prepare Al-20%Mg with fine aluminium, pure silicon and Al-Mg alloy
2The Si alloy, 750 ℃ of synthesis temperatures, preparation process induction stirring magnetic field parameter is 30Hz, electric current 150A.The pulsewidth of process of setting pulsed magnetic field is 100ms, and pulsed magnetic field intensity is 2T, and stripping speed is 10cm/min, makes 20%Mg
2The Si particle enhanced aluminum-based composite material.
Fig. 4 applies pulsed magnetic field front and back Mg
2The solidified structure of Si particle enhanced aluminum-based composite material and XRD detected result.As seen from the figure: (1) is α (Al) and Mg by the type that XRD figure draws phase in the solidified structure
2The Si phase; (2) under the alloying constituent same case, apply Mg behind the pulsed magnetic field
2The Si particle generates quantity to be increased, and particle size is reduced to 10～25 μ m by 30～50 μ m, and thinning effect is obvious, and the particle size degree of uniformity improves, and the homogenizing degree that distributes in matrix improves; (3) α (Al) is mutually fined, and promptly the matrix metal grain-size reduces, and the average grain size when not applying pulsed magnetic field is at 100～120 mu m ranges, apply pulsed magnetic field after average grain size refine to 40～60 μ m.Comprehensively it seems: apply in the process of setting that the solidified structure of matrix material is able to obvious improvement behind the pulsed magnetic field.
In-situ crystallization technique prepares 10%Mg under embodiment 4 pulsed magnetic fields
2The Si particle enhanced aluminum-based composite material
Prepare Al-10%Mg with fine aluminium, pure silicon and Al-Mg alloy
2The Si alloy, 700 ℃ of synthesis temperatures, preparation process induction stirring magnetic field parameter is 30Hz, electric current 120A.The pulsewidth of process of setting pulsed magnetic field is 150ms, and pulsed magnetic field intensity is 1T, and stripping speed is 10cm/min, makes 10%Mg
2The Si particle enhanced aluminum-based composite material.
Fig. 5 applies pulsed magnetic field front and back 10%Mg
2The solidified structure of Si particle enhanced aluminum-based composite material and spectroscopy detection result.As seen from Figure 5: (1) by the energy spectrum analysis figure of particle phase as seen, in the solidified structure type of phase be α (Al) with AlMgSi mutually (analytic target be Fig. 5 (a) (b) shown in the rounding particle), in view of Mg in the grain fraction: Si=2: 1 (atomic ratio), then decidable is that particle is Mg mutually
2Si; (2) under the alloying constituent same case, apply Mg behind the pulsed magnetic field
2The Si particle generates quantity to be increased, and particle size is reduced to 20～30 μ m by 30～50 μ m, though thinning effect is not fairly obvious, visible particle generates quantity obviously to be increased, and size is even, and the homogenizing degree that distributes in matrix improves; (3) α (Al) is mutually fined, and promptly the matrix metal grain-size reduces, and the average grain size when not applying pulsed magnetic field is at 100～120 mu m ranges, apply pulsed magnetic field after average grain size refine to 50～60 μ m.Comprehensively it seems: apply in the process of setting that the solidified structure of matrix material is able to obvious improvement behind the pulsed magnetic field.
Claims (6)
1. pulsed magnetic field prepare down the method for high-performance aluminum-base composite material, it is characterized in that: the aluminum matrix composite melt after synthesizing under the induction stirring the action of a magnetic field, solidification and crystallization under pulsed magnetic field.
2. the described preparation method of claim 1, it is characterized in that: aluminum matrix composite melt synthetic technology under the induction stirring the action of a magnetic field is: earlier aluminum or aluminum alloy is melted, the composition of determining alloy melt according to the wild phase volume fraction of wild phase kind and requirement carries out alloying, the alloying temperature is determined according to element solubleness and alloy melting temperature, the alloying temperature is higher 10～200 ℃ than alloy melt liquidus temperature, strengthens body and can select Si phase, Al
3Ti or Mg
2Si, matrix are mainly Al or Al base alloy; The synthetic preparation process of compounding flux melting adopts induction stirring, and the intensity of induction stirring is as the criterion not destroy weld pool surface insulating covering agent or oxidation film layer.
3. the described preparation method of claim 2, it is characterized in that: the frequency-tuning range in induction stirring magnetic field is 1～30Hz, and the strength of current regulation range is: 100～750A.
4. the described preparation method of claim 1, it is characterized in that: the technology that Composite Melt is solidified under pulsed magnetic field is: the pulsewidth of pulsed magnetic field is 1～500ms, pulsed magnetic field amplitude intensity 0.1～50T.
5. pulsed magnetic field prepares the device of high-performance aluminum-base composite material down, comprise induction stirring magnetic field (1), heating system (2), melting synthesis reactor (3), control stream stopper (or chute baffle plate) (4), following water filling port (or chute) (6), thermometric and temperature controlling system (7), casting is pushed up (8) with heat, bed die and stripping device (12), pulsed magnetic field apparatus (14) and level monitoring and control (15), it is characterized in that: be provided with the solidification and crystallization device with below, heat top (8) in casting, crystallizer is divided into three sections from top to bottom: special crystallizer pottery section (9), special crystallizer graphite annulus section (10) and special crystallizer fine copper section (11), the height ratio between three sections is 1: 2: 1.
6. the described device of claim 5, it is characterized in that: the center of special crystallizer graphite annulus section (10) and the hub of a spool of pulsed magnetic field coil are at sustained height.
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