CN101704075B - Method for synthesizing aluminum-based composite material by multielement magnetic field combined fusant reaction - Google Patents
Method for synthesizing aluminum-based composite material by multielement magnetic field combined fusant reaction Download PDFInfo
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Abstract
The invention relates to a method for synthesizing an aluminum-based composite material by multielement magnetic field combined fusant reaction, which belongs to the technical field of preparation of materials. In the method, the fusant reaction synthesizing process is divided into three phases of reactant dispersion, contact chemical reaction and reaction product dispersion and by-product separation according to the characteristic that the fusant synthesizing reaction is solid-liquid phase reaction; and a corresponding combined magnetic field is applied according to different characteristics of all phases to carry out control. A high-frequency magnetic field and a low-frequency traveling wave magnetic field are applied in the reactant dispersion phase to improve the dispersing effect and the dispersing rate of a reactant; a pulse magnetic field and the low-frequency traveling wave magnetic field are applied in the contact reaction phase to accelerate the in-situ reaction course in a fusant; and the high-frequency magnetic field and the pulse magnetic field are applied in the reaction product dispersion and by-product discharge phase to control the clustering of particles and be beneficial to separating slag phases. The method can realize accurate control on the reaction synthesizing process of the fusant, improves the synthesizing efficiency and is beneficial to improving the quality of the composite material fusant.
Description
Technical field
The present invention relates to the preparing technical field of particle enhanced aluminum-based composite material, specially refer to a kind of polynary combination field method synthetic of utilizing the fusant reaction of aluminum matrix composite.
Background technology
Particle enhanced aluminum-based composite material becomes a kind of application new material more and more widely gradually because of having compound architectural feature and good physics and chemistry and mechanical performance.At present, the fusant reaction synthetic method is the important method of preparation particle enhanced aluminum-based composite material, and this method is by adding reactant in melt, forms by reactant and in-situ chemical reaction between aluminum substrate and strengthens particle mutually.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 synthetic process control of fusant reaction 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-situ building-up process to melt applies the magnetic field of being made up by rotating excitation field and travelling-magnetic-field, this invention can improve solid-phase reactant and generate the dispersiveness of particle, thereby improve the dynamic conditions of reaction, but the deficiency of this invention is the combination field that is applied, all be low frequency magnetic field (＜100Hz), because the energy of low frequency magnetic field is low and dispersion, so magnetic field energy is the mechanical energy based on stirring, to the not influence of fluctuation of energy of chemical reaction, just can not change the thermodynamic condition of solid-liquid phase reaction.Proposing building-up process in position applies the prior art that low frequency magnetic field stirs and also has: Chinese patent: CN 101199989, the alien frequencies composite electromagnetic is the method for continuous casting particulate reinforced metal matrix composite after the match, Chinese patent: CN 1667147C, a kind of preparation method of endogenous particle reinforced aluminium-based composite material.Above prior art applies a kind of low frequency magnetic field of form to the whole process of fusant reaction, and this magnetic field is very little to the thermodynamics influence of recombination reaction, even not effect, is not that different phase adopts different magnetic field effects according to the process of reaction in-situ also.
Chinese patent: CN 101391290A, a kind of magnetic field and ultrasonic field coupling prepare the method for metal-base composites down, the process that proposes reaction in position applies magnetic field and ultrasonic coupled field, there are three kinds of schemes in the magnetic field that is proposed, comprise: strong pulsed magnetic field, higher-order of oscillation magnetic field and low frequency alternating magnetic field, three kinds of magnetic fields that this invention is mentioned are three kinds of proposing at different preparation purpose and the technical scheme of ultrasonic field coupling, its deficiency is: electromagnetic field belongs to electromagnetic wave, and ultrasonic field belongs to mechanical wave, the action effect of two kinds of fields can be complementary, the coupling but two kinds of different fields can not superpose, so this scheme essence is the coupling and complementing of the effect of single magnetic field and two kinds of effects of ultrasonication, in addition, this invention is not that different phase adopts different magnetic field effects according to the process of reaction in-situ also, the effect in different outfields is not given full play to.
Because the fusant reaction building-up process is typical solid-liquid phase reaction, characteristics according to solid-liquid phase reaction, its reaction mechanism is promptly reacted and is formed link for can mainly be divided into for three steps: one, the dispersion of reactant and to the mass transport process of solid-liquid interface, and this mainly is a kinetics problem; Two, on the solid liquid interface chemical reaction takes place, generate particle phase particle, this mainly is a thermodynamics of reactions problem; Three, the discharge of the growing up of the particle phase that generates of reaction, diffusion and byproduct of reaction, this relates in the melt cenotype and separates out the thermodynamics and kinetics of growing up, but mainly can be regarded as the process based on dynamics.In view of the fusant reaction building-up process in the different stages, the physical chemistry problem difference that relates to, so, if apply a kind of single outfield or compound outfield in whole fusant reaction building-up process, then can not give full play to the effect in outfield, also not reach the purpose of utilizing the outfield accurately to control the fusant reaction building-up process.
In sum, the synthetic process control of fusant reaction is the key that melting-reaction method prepares particle enhanced aluminum-based composite material, the existing outfield of adopting comprises that magnetic field, ultrasonic wave and compound the technology of controlling or improve reaction condition are not this key characters of solid-liquid phase reaction according to the fusant reaction synthetic method, takes suitable outfield to control according to reactions steps and process.Therefore, according to the mechanism of fusant reaction building-up process, design is fit to the outfield in differential responses stage, and the reaction building-up process is controlled, and is significant to the preparation of high-performance composite materials.
Summary of the invention
The objective of the invention is to prepare the building-up process mechanism of particulate reinforced composite according to melting-reaction method, in the synthetic different phase of reaction, apply multi-form magnetic field, the original position building-up process is accurately controlled, make each link of building-up process all reach optimum reaction condition, realize optimum response efficient and bring into play the control action of outfield to greatest extent the fusant reaction process.
The objective of the invention is to realize by following technical proposal:
According to the fusant reaction building-up process is typical solid-liquid phase reaction, and according to the characteristics of solid-liquid phase reaction, its reaction is formed link for can mainly be divided into three phases, applies different magnetic field according to the characteristics in each stage of building-up process and controls.
Phase I: this stage is the dispersion of reactant and the reactant mass transport process to solid-liquid interface, this is a kinetics problem, the purpose that this stage applies magnetic field is to promote the dispersion of reactant and accelerate the process of reactant to the solid-liquid interface mass transfer, according to boundary layer theory and surface renewal theory, the integral body that should strengthen melt stirs to promote the dispersion of reactant, simultaneously, improve disturbance to melt, to improve the wetability of reactant and melt, promote the mass transport process of reactant to solid-liquid interface.
Therefore this stage applies a kind of combination field, and this combination field is by low frequency magnetic field and high frequency magnetic field combination, and low frequency magnetic field is realized the integral body of melt is stirred, and high frequency magnetic field is realized the disturbance to melt.
The low frequency magnetic field that this stage applies combination field is the low frequency travelling-magnetic-field, and the electromagnetic parameter scope that is adopted is: frequency 1～100Hz, electric current 100～1000A determines optimum frequency and current value by stirring intensity.
The electromagnetic parameter scope that the high frequency magnetic field of combination field that this stage applies adopts is: frequency 1kHz～30kHz, electric current 10～500A presents tangible disturbance with melt and determines optimum frequency and current value.
Second stage: this stage is to take place the chemical reaction stage on the solid-liquid interface, generates particle phase particle, and this mainly is a thermodynamics of reactions problem.According to the thermodynamic principles of chemical reaction, want to improve the speed of reaction, can take two kinds of approach: the one, improve the temperature of reaction, the 2nd, reduce the activation energy of reaction, provide energy with the form in outfield to the reaction particle.Owing to improve reaction temperature, be limited by technological factor, the temperature of melt is high more, and it is air-breathing, the oxidation of metal etc. is serious more, so the fusant reaction synthesis temperature is difficult for too high.Therefore, this stage can be used pulsed magnetic field, utilizes the energy in magnetic field to reduce the activation energy of reaction in-situ, so only introduce pulsed magnetic field, be because utilize pulse technique, can make magnetic field in short-term, reach very high intensity, directly the atomic scale of effect and material.Even for the reaction that guarantees the molten bath, apply magnetic field simultaneously melt is carried out the integral body stirring.
Therefore, this stage applies a kind of combination field, and this combination field is by pulsed magnetic field and low frequency magnetic field combination, pulsed magnetic field is used to reduce reaction activity, with the raising reaction rate, and low frequency magnetic field is realized the integral body of melt is stirred, and guarantees the macro-uniformity of melt tank reaction.
The electromagnetic parameter scope that the pulsed magnetic field of combination field that this stage applies adopts is: pulse current frequency 0.01～20Hz, inductor central magnetic field intensity 0.5～20T.
The low frequency magnetic field that this stage applies combination field is the low frequency travelling-magnetic-field, and the electromagnetic parameter scope that is adopted is: frequency 1～100Hz, electric current 100～1000A determines optimum frequency and current value by stirring intensity.
Phase III: this stage is the discharge stage of the growing up of the particle phase that generates of reaction, diffusion and byproduct of reaction, and this stage will be controlled growing up of particle phase and cluster, realizes the dispersion of particle phase, will help the discharge that byproduct of reaction is the slag phase simultaneously.
Therefore, this stage applies a kind of combination field, and this combination field is by pulsed magnetic field and high frequency magnetic field combination, pulsed magnetic field is used to control the cluster of particle phase, it is disperseed, and this is to utilize the short-time pulse electromagnetic force of pulsed magnetic field that particle is disperseed, and suppresses the cluster of particle phase and grows up.High frequency magnetic field is realized the disturbance to melt, helps the discharge of accessory substance, also helps the dispersion of particle phase simultaneously.
The electromagnetic parameter scope that the pulsed magnetic field of combination field that this stage applies adopts is: pulse current frequency 0.01～20Hz, inductor central magnetic field intensity 0.5～20T.
The electromagnetic parameter scope that the high frequency magnetic field of combination field that this stage applies adopts is: frequency 1kHz～30kHz, electric current 10～500A presents significantly disturbance with melt and determines optimum frequency and current value.
Compared with prior art the present invention has the following advantages and effect:
1) the present invention is according to the characteristics and the reaction mechanism of fusant reaction process, different phase in reaction applies different combination fields, realization all adopts a kind of single magnetic field or a kind of combination field more effective than prior art in whole fusant reaction process to effective control of reaction building-up process;
2) the reactant scatter stage applies the magnetic field of high frequency+low frequency combination, realizes that simultaneously the integral body of melt stirs and the microcell vibration, has more effectively improved the rate of dispersion and the disperse effect of reactant;
3) contact pulsed magnetic field+low frequency travelling-magnetic-field that the chemical reaction stage applies, reduced reaction activity, thereby improved reaction in-situ speed, the integral body of low frequency travelling-magnetic-field stirs the uniformity that has guaranteed melt tank reaction;
4) pulsed magnetic field that particle disperses mutually and the byproduct of reaction discharge stage applies and high frequency magnetic field have suppressed the cluster of particle phase and have grown up, and make it that good dispersiveness be arranged, and simultaneously, high frequency magnetic field impels the disturbance of melt, and helping byproduct of reaction is the separation of slag phase;
Therefore, the present invention is directed to the different phase of fusant reaction process, adopt multi-form combination field to control, improved the speed of each link of fusant reaction building-up process, effectively shorten generated time, improve the utilization rate and the recovery rate of reactant simultaneously, and reduced the possibility of melt slag inclusion, realized the preparation of high-performance particulate reinforced composite melt.
Description of drawings
The combination of Fig. 1 multielement magnetic field is fusant reaction synthesizing aluminum-based composite material schematic diagram down
A phase I combination field, B second stage combination field, C phase III combination field
1 high frequency magnetic field; 2 travelling-magnetic-fields; 3 pulsed magnetic fields;
The sem photograph of Fig. 2 embodiment 1 preparation material
The sem photograph of Fig. 3 embodiment 2 preparation materials
The specific 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
Raw material: parent metal: commercial-purity aluminium; Pressed powder: industrial carbonic acid zirconium (Zr (CO
3)
2) pulvis (purity is 99.20%), the refining degasser and the agent of skimming;
Reaction in-situ equation: 7Al
(l)+ Zr (CO
3)
2 (s)=Al
3Zr
(s)+ 2Al
2O
3 (s)
Particle wild phase: Al
3Zr
(s)And Al
2O
3 (s)
Preparation process is as follows:
(1) at first carry out the preparation of Metal Melting and powder:
Commercial-purity aluminium 10Kg melts in 25kW crucible type resistance furnace and is warmed up to 870 ℃, 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% (annotate: the theoretical volume mark of particle phase is about 13.68vol%) 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 fusant reaction synthesizer of molten metal impouring band heat insulation function of temperature requirement (870 ℃) in refining, in melt, be pressed into solid reactant Zr (CO with bell jar
3)
2Powder.
(a) shown in Figure 1A, open 2 pairs of melts of high frequency magnetic field 1 and low frequency travelling-magnetic-field and stir, disperse reactant, the frequency 20kHz of high frequency magnetic field, electric current 80A, the frequency 15Hz of low frequency travelling-magnetic-field, electric current 250A.The magnetic field effect was closed high frequency magnetic field after 2 minutes;
(b) shown in Figure 1B, unbalanced pulse magnetic field 3, the parameter in regulating impulse magnetic field is frequency 1Hz, inductor central magnetic field intensity 5T, the frequency 10Hz of low frequency travelling-magnetic-field, electric current 150A.Low frequency travelling-magnetic-field 2 is closed in the magnetic field effect after 10 minutes;
(b) shown in Fig. 1 C, open high frequency magnetic field 1, the parameter in regulating impulse magnetic field is frequency 20kHz, electric current 80A, the electromagnetic parameter of pulsed magnetic field is constant, after 3 minutes, closes all magnetic fields, and melt prepares.
(3): metal pours in the metal pattern die, makes composite castings, sample analysis, dense internal organization, solidified structure defectives such as nothing is loose, shrinkage cavity, particle size 0.5～1 μ m, belong to the submicron particles reinforced composite, the as-cast structure sem photograph of material as shown in Figure 2.
Use the outstanding feature of this invention to be: the reaction time shortened to 20 minutes from 30 minutes, the rate of the receipts of reactant improves, when being embodied in same reaction thing addition, the content of composite material granular phase increases behind employing the present invention, in addition, the particle size uniformity improves, and does not have obvious cluster phenomenon, and the grain refine effect is arranged.
Be actual effect more of the present invention, with prior art as a comparison case, the selection of Comparative Examples sees Table 1, and method of the present invention is as shown in table 2 compared with the prior art.
The Comparative Examples that table 1 is selected
| Comparative Examples 1 | Chinese patent CN101391291A title: the method for metal matrix composition home-position synthesizing under a kind of combined electric magnetic field |
| Comparative Examples 2 | Chinese patent: CN 101199989 titles: the alien frequencies composite electromagnetic is the method for continuous casting particulate reinforced metal matrix composite after the match |
| Comparative Examples 3 | Chinese patent: CN 1667147C title: a kind of preparation method of endogenous particle reinforced aluminium-based composite material |
| Comparative Examples 4 | Chinese patent: CN 101391290A title: a kind of magnetic field and ultrasonic field coupling prepare the method for metal-base composites down |
Table 2 adopts the comparison of embodiments of the invention 1 and Comparative Examples
Raw material: parent metal: pure Al; Reacting salt: K
2ZrF
6-KBF
4(mass fraction was than 6.2: 7.8) salt-mixture pulvis, the refining degasser and the agent of skimming;
Preparation process is as follows:
(1) at first carry out the preparation of Metal Melting and powder:
The pure Al of the 2Kg crucible of packing into, fusing is warmed up to 900 ℃ in the 25kW resistance furnace, outgases, skims.Agents useful for same is all fully dried down at 250 ℃～300 ℃, wherein K
2ZrF
6-KBF
4, grinding to form fine powder (granularity is less than 200 orders), the weight that salt-mixture adds is 20% of weight metal.
(2): the multielement magnetic field combination is the preparation Composite Melt down:
Refining is good and meet temperature and reach 900 ℃, with bell jar with K
2ZrF
6-KBF
4Be pressed in the aluminium liquid in the crucible, crucible is put into magnetic sensors.
(a) shown in Figure 1A, open 2 pairs of melts of high frequency magnetic field 1 and low frequency travelling-magnetic-field and stir, disperse reactant, the frequency 10kHz of high frequency magnetic field, electric current 40A, the frequency 10Hz of low frequency travelling-magnetic-field, electric current 150A.The magnetic field effect was closed high frequency magnetic field after 2 minutes;
(b) shown in Figure 1B, unbalanced pulse magnetic field 3, the parameter in regulating impulse magnetic field is frequency 2Hz, inductor central magnetic field intensity 5T, the frequency 5Hz of low frequency travelling-magnetic-field, electric current 100A.Low frequency travelling-magnetic-field 2 is closed in the magnetic field effect after 10 minutes;
(b) shown in Fig. 1 C, open high frequency magnetic field 1, the parameter in regulating impulse magnetic field is frequency 10kHz, electric current 40A, the electromagnetic parameter of pulsed magnetic field is constant, after 3 minutes, closes all magnetic fields, and melt prepares.
Melt leaves standstill, and treats that temperature drops to 730 ℃, and 720 ℃ of water cooled copper moulds that pour into water-cooled diameter 200mm obtain the circle base.
Composite Melt has good flowability, and the composite strand outer surface that makes is bright and clean, dense internal organization, and solidified structure defectives such as nothing is loose, shrinkage cavity, particle size 0.2～1 μ m, the as-cast structure sem photograph of material is as shown in Figure 3.
Use the outstanding feature of this invention to be: the reaction time shortened to 20 minutes from 30 minutes, and the rate of the receipts of reactant improves more than 15%, and in addition, the particle size uniformity improves, and does not have obvious cluster phenomenon, and the grain refine effect is arranged, and particle size is less than 1 μ m.
Be actual effect more of the present invention, make Comparative Examples with the prior art that table 1 provides, method of the present invention is as shown in table 3 compared with the prior art.
Table 3 adopts the comparison of embodiments of the invention 2 and Comparative Examples
Claims (7)
1. the method for synthesizing aluminum-based composite material by multielement magnetic field combined fusant reaction, it is characterized in that: the fusant reaction building-up process is divided into reactant disperses, contact chemical reaction and product dispersion and accessory substance discharge three phases, according to the different characteristics in each stage, apply corresponding combination field and control; Apply high frequency magnetic field+low frequency travelling-magnetic-field at the reactant scatter stage and improve reactant dispersion effect and speed; Apply pulsed magnetic field and low frequency travelling-magnetic-field the chemical reaction stage to quicken reaction in-situ process in the melt in contact; Disperse and the accessory substance discharge stage applies high frequency magnetic field and pulsed magnetic field in product, control particle phase cluster and help slag to be separated.
2. the method for synthesizing aluminum-based composite material by multielement magnetic field combined fusant reaction as claimed in claim 1, it is characterized in that: the electromagnetic parameter scope that applies the low frequency travelling-magnetic-field at the reactant scatter stage is: frequency 1～100Hz, electric current 100～1000A.
3. the method for synthesizing aluminum-based composite material by multielement magnetic field combined fusant reaction as claimed in claim 1 is characterized in that: applying the electromagnetic parameter scope that high frequency magnetic field adopts at the reactant scatter stage is: frequency 1kHz～30kHz, electric current 10～500A.
4. the method for synthesizing aluminum-based composite material by multielement magnetic field combined fusant reaction as claimed in claim 1 is characterized in that: the electromagnetic parameter scope that applies the low frequency travelling-magnetic-field in the contact chemical reaction stage is: frequency 1～100Hz, electric current 100～1000A.
5. the method for synthesizing aluminum-based composite material by multielement magnetic field combined fusant reaction as claimed in claim 1, it is characterized in that: the electromagnetic parameter scope that applies the pulsed magnetic field employing in the contact chemical reaction stage is: pulse current frequency 0.01～20Hz, inductor central magnetic field intensity 0.5～20T.
6. the method for synthesizing aluminum-based composite material by multielement magnetic field combined fusant reaction as claimed in claim 1, it is characterized in that: in the electromagnetic parameter scope that product is disperseed and the accessory substance discharge stage applies the high frequency magnetic field employing be: frequency 1kHz～30kHz, electric current 10～500A.
7. the method for synthesizing aluminum-based composite material by multielement magnetic field combined fusant reaction as claimed in claim 1, it is characterized in that: in the electromagnetic parameter scope that product is disperseed and the accessory substance discharge stage applies the pulsed magnetic field employing be: pulse current frequency 0.01～20Hz, inductor central magnetic field intensity 0.5～20T.
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| CN102069175B (en) * | 2011-01-24 | 2013-01-02 | 哈尔滨工业大学 | Plug-in cylindrical traveling wave magnetic field sensor for casting |
| CN106756192A (en) * | 2016-12-16 | 2017-05-31 | 镇江创智特种合金科技发展有限公司 | A kind of magnetochemistry method for preparing super modeling aluminum matrix composite in situ |
| CN108339963B (en) * | 2018-03-29 | 2019-07-30 | 东北大学 | A kind of difference phase travelling-magnetic-field electromagnetic casting method |
| CN110076309B (en) * | 2019-06-13 | 2020-06-30 | 中南大学 | Electric pulse device and method for locally regulating and controlling phase state distribution of covering slag in slag channel of continuous casting crystallizer |
| CN111041288B (en) * | 2019-12-18 | 2021-10-12 | 江苏大学 | High-toughness anti-fatigue in-situ aluminum-based composite material and preparation method thereof |
| CN115232999B (en) * | 2022-07-19 | 2023-03-14 | 西北工业大学 | Preparation method and system of electromagnetic suspension material |
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| CN1093628A (en) * | 1993-04-10 | 1994-10-19 | 中国科学院金属研究所 | The electromagnetic stirring casting technology of metal-base composites |
| CN101391291A (en) * | 2008-11-05 | 2009-03-25 | 江苏大学 | Metal matrix composition home-position synthesizing method in combined electric magnetic field |
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2009
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| US4828015A (en) * | 1986-10-24 | 1989-05-09 | Nippon Steel Corporation | Continuous casting process for composite metal material |
| CN1093628A (en) * | 1993-04-10 | 1994-10-19 | 中国科学院金属研究所 | The electromagnetic stirring casting technology of metal-base composites |
| CN101391291A (en) * | 2008-11-05 | 2009-03-25 | 江苏大学 | Metal matrix composition home-position synthesizing method in combined electric magnetic field |
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Application publication date: 20100512 Assignee: Danyang Rongjia Precision Machinery Co., Ltd. Assignor: Jiangsu University Contract record no.: 2016320000060 Denomination of invention: Method for synthesizing aluminum-based composite material by multielement magnetic field combined fusant reaction Granted publication date: 20111221 License type: Exclusive License Record date: 20160229 |
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