CN102134667A - Preparation method of submicron particle-reinforced aluminum-based composite material - Google Patents

Preparation method of submicron particle-reinforced aluminum-based composite material Download PDF

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Publication number
CN102134667A
CN102134667A CN 201110047197 CN201110047197A CN102134667A CN 102134667 A CN102134667 A CN 102134667A CN 201110047197 CN201110047197 CN 201110047197 CN 201110047197 A CN201110047197 A CN 201110047197A CN 102134667 A CN102134667 A CN 102134667A
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China
Prior art keywords
magnetic field
melt
energy ultrasonic
reaction
preparation
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CN 201110047197
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Chinese (zh)
Inventor
赵玉涛
董洪标
张钊
陈登斌
陈刚
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JIANGSU C &E MATERIALS RESEARCH INSTITUTE Co Ltd
Jiangsu University
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JIANGSU C &E MATERIALS RESEARCH INSTITUTE Co Ltd
Jiangsu University
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Priority to CN 201110047197 priority Critical patent/CN102134667A/en
Publication of CN102134667A publication Critical patent/CN102134667A/en
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Abstract

The invention provides a preparation method of a submicron particle-reinforced aluminum-based composite material, belonging to the technical field of preparation of metal-based composite materials. The method comprises the steps of: refining an aluminum melt or an aluminum alloy melt and then adjusting to a reaction starting temperature; adding a reactant which can have in-situ reaction with the aluminum melt or the aluminum alloy melt to generate particle phase so as to carry out synthetic reaction; applying high-energy ultrasound and low-frequency stirring magnetic field during the synthetic reaction; and standing to a pouring temperature and carrying out pouring after the reaction is finished, wherein the high-energy ultrasound and low-frequency stirring magnetic field are applied at the same time and the high-energy ultrasound is applied intermittently. When an intermittent application manner is adopted, the service life of a amplitude transformer can be prolonged and the quality deterioration of the melt caused by the introduction of impurity elements due to the corrosion of the amplitude transformer is prevented; and the size of the generated particles is smaller than that generated by other manners so that the manner has the function of thinning and reinforcing the particles and is beneficial to improvement of the mechanical property of the submicron particle-reinforced aluminum-based composite material.

Description

A kind of preparation method of sub-micron granule strengthening aluminum base composite material
Technical field
The present invention relates to the preparing technical field of particle enhanced aluminum-based composite material, specially refer to a kind of preparation method of sub-micron granule strengthening aluminum base composite material.
Background technology
Aluminum matrix composite has high specific tenacity, specific rigidity, the excellent high-temperature mechanical property, low thermal expansivity and good advantages such as wear resistance are in aerospace, automobile, electronics, optics, fields such as physical culture have very wide application prospect, to strengthen the body cost low because of it has for particle enhanced aluminum-based composite material, microtexture is even, the material property isotropy, advantage such as can adopt that traditional metal working process is processed, has the suitability for industrialized production prospect, receive much attention especially, particularly use the matrix material of reaction in synthetic technology preparation, because enhanced granule forming core from matrix is grown up, has Heat stability is good, particle is tiny, be evenly distributed, with advantage such as matrix bond is good, remedied that to add the enhanced granule size big, a series of shortcomings such as interfacial bonding property difference, be considered to be hopeful to realize the new technology of industrial applications, but there are enhancing bodily form looks in this technology, size, shortcomings such as it is wayward to distribute, thereby limited this Industrial Application of Technology.
Utilization adds thermodynamics and the dynamic conditions that physical field improves reaction, pattern, size, distribution that the control particulate reinforced composite strengthens body have had relevant patent, are that the Chinese patent of CN101391290A has provided a kind of method that fusant reaction synthesizes metal-base composites under magnetic field and the ultrasonic field coupling of utilizing such as patent publication No..But this method is defined as coupling to two kinds of physical fields, has greatly limited the flexible Application for specific system, in addition, under magnetic field and the ultrasonic field coupling horn high-temperature corrosion resistance is had higher requirement.
In order to remedy above-mentioned deficiency, the present invention proposes to adopt the method for high-energy ultrasonic and magnetic field synergy reaction synthesizing submicron particle enhanced aluminum-based composite material.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of sub-micron granule strengthening aluminum base composite material is with preparation high performance submicron particle enhanced aluminum-based composite material.
Ultimate principle of the present invention is: apply low frequency in position in the reaction process of aluminum matrix composite simultaneously and stir magnetic field and high-energy ultrasonic field, utilize magnetic field melt to be produced sonochemistry principles such as acoustic cavitation that the hot equimagnetic principles of chemistry of electromagnetic force, magnetization and vortex induction and high-energy ultrasonic field produce and acoustic streaming impact in melt the synthetic preparation process of matrix material acted synergistically, reach control particle phase distribution, suppress that particle is grown up and cluster and change the purpose of the thermodynamics and kinetics condition of in-situ synthesized reaction.
Difference according to Composite Melt preparation method and reaction system, can select different magnetic field to apply form, magnetic field herein is that low frequency stirs magnetic field, when selecting low frequency magnetic field and high-energy ultrasonic synergy for use, its principle is: high-energy ultrasonic is by empty effect of sound and acoustic streaming shock effect in the melt, the enhancing body particle that generates in the greatly refinement reaction process, and the reunion that may exist bunch is scattered, the acoustic streaming effect plays stirring action to microcell, and the direction of its stirring movement is vertical, promptly be parallel to the horn direction, and the low frequency that adds stirs the direction of motion of its stirring of magnetic field for laterally, promptly perpendicular to the horn direction, and the stack of these two kinds of motions, just obtained the stirring of 3 D stereo, particulate has been disperseed to have played active effect.
Based on above-mentioned principle, realize that technical scheme of the present invention is:
The novel method of a kind of high-energy ultrasonic and magnetic field synergy reaction synthesizing submicron particle enhanced aluminum-based composite material: will adjust to reacting initial temperature after molten aluminium or the aluminium alloy melt refining, adding can generate particle reactant mutually with molten aluminium or aluminium alloy melt reaction in and carry out building-up reactions, in synthetic reaction process, apply high-energy ultrasonic and low frequency and stir magnetic field, question response finishes, and leaves standstill to pour into a mould after reducing to teeming temperature.
Low frequency stirs magnetic field and applies in the outside in reaction molten bath, and low frequency stirs the magnetic field preferred parameter and is: frequency 3Hz, electric current 150A; The high-energy ultrasonic preferred parameter is: frequency 20kHz, ultrasound intensity 0.8kW/cm 2~ 1.2kW/cm 2, the mode that high-energy ultrasonic applies is that ultrasonic amplitude transformer is reached 5mm ~ 6mm under the melt liquid level.
It can be that two kinds of physical fields are earlier after-applied separately that high-energy ultrasonic and low frequency stir the synergistic form in magnetic field, also can be to apply simultaneously; When applying simultaneously, high-energy ultrasonic can be to apply continuously or intermittent type applies, application time 3 ~ 5 minutes; When two kinds of physical fields were earlier after-applied separately, the time that low frequency stirring magnetic field applies was 3~5 minutes; The time that high-energy ultrasonic applies is 5~8 minutes.
Comparing advantage of the present invention with the sound magnetic coupling interaction is:
Applying of (1) two kind of physical field has handiness more, at reaction system and preparation method not
With, the synergy form of physical field with apply mode and can arrange in pairs or groups flexibly;
(2) when adopting intermittent type to apply mode, the high temperature resistant corruption that can improve horn greatly
Erosion property in the work-ing life that not only can improve horn, can prevent that more the melt quality that the introducing of the impurity element that causes because of the horn corrosion causes from worsening;
(3) high-energy ultrasonic and low frequency stir that magnetic field applies simultaneously and high-energy ultrasonic intermittent type when applying, application time 30~50 seconds, 30~50 seconds intermittent times, the particle size that generates is littler than other modes, illustrate that this kind mode has the effect of refinement enhanced granule, helps improving the mechanical property of described sub-micron granule strengthening aluminum base composite material.
Embodiment
The invention will be further elaborated below in conjunction with embodiment:
Embodiment 1:
With ZrO 2+ B 2O 3(Zr, B mol ratio 1:2) powder is through 150 ~ 200 ℃ of oven dry 2h, with standby after the grinding of the powder after the baking, the screening.After 7055 aluminum alloy ingots melt, add the anti-oxidation of insulating covering agent protection in molten aluminium stove, be warmed up to 900 ℃, the desurfacing coverture is with the ZrO of aluminum alloy melt quality 2wt% 2+ B 2O 3Powder coats with aluminium foil and joins in the aluminium alloy melt, starts low frequency and stirs magnetic field, and magnetic field parameter is frequency 3Hz, electric current 150A; After treating that magnetic field is stable, ultrasonic amplitude transformer is reached 5mm under the melt liquid level, the high-energy ultrasonic parameter is frequency 20kHz, ultrasound intensity 0.8kW/cm 2, common continuous action 3min, reaction finishes the back cooling; refining; skim, add the anti-oxidation of insulating covering agent protection simultaneously, when melt temperature reaches teeming temperature, pour in the water cooled copper mould of diameter 100mm; obtain the matrix material ingot casting; Composite Melt has good flowability, and the matrix material strand outside surface that makes is bright and clean, dense internal organization; solidified structure defectives such as nothing is loose, shrinkage cavity, particle size 0.5 ~ 1 μM.
Embodiment 2:
Other preparation conditions are constant; high-energy ultrasonic changed into intermittently apply; every 30s horn is taken out from melt; intermittently apply once more behind the 30s and reach 3min until the accumulative total application time; reaction finishes the back cooling; refining; skim, add the anti-oxidation of insulating covering agent protection simultaneously, when melt temperature reaches teeming temperature, pour in the water cooled copper mould of diameter 100mm; obtain the matrix material ingot casting; Composite Melt has good flowability, and the matrix material strand outside surface that makes is bright and clean, dense internal organization; solidified structure defectives such as nothing is loose, shrinkage cavity, particle size 0.2 ~ 0.4 μM.
Embodiment 3:
With B 2O 3+ K 2ZrF 6(Zr, B mol ratio 1:1) powder is through 150 ~ 200 ℃ of oven dry 2h, with standby after the grinding of the powder after the baking, the screening, after 7055 aluminum alloy ingots melt in molten aluminium stove; add the anti-oxidation of insulating covering agent protection; be warmed up to 900 ℃, the desurfacing coverture is with the B of aluminum alloy melt quality 5wt.% 2O 3+ K 2ZrF 6Powder coats with aluminium foil and joins in the aluminium alloy melt, starts low frequency and stirs magnetic field, and magnetic field parameter is frequency 3Hz, electric current 150A; Close magnetic field behind the action of a magnetic field 3min, ultrasonic amplitude transformer is reached 5mm ~ 6mm under the melt liquid level, the high-energy ultrasonic parameter is frequency 20kHz, ultrasound intensity 1.2kW/cm 2, applying ultrasonic field 7min, reaction finishes the back cooling; refining; skim, add the anti-oxidation of insulating covering agent protection simultaneously, when melt temperature reaches teeming temperature, pour in the water cooled copper mould of diameter 100mm; obtain the matrix material ingot casting; Composite Melt has good flowability, and the matrix material strand outside surface that makes is bright and clean, dense internal organization; solidified structure defectives such as nothing is loose, shrinkage cavity, particle size 0.6 ~ 1 μM.
Embodiment 4
Other preparation conditions are constant, and high-energy ultrasonic and low frequency stir that magnetic field applies simultaneously and high-energy ultrasonic intermittent type when applying, and the time that applies is 5 minutes; Every 30s horn is taken out from melt for the first time; intermittently apply once more behind the 50s; every 40s horn is taken out from melt for the second time; intermittently apply once more behind the 30s; every 40s horn is taken out from melt for the third time; intermittently apply once more behind the 50s; the 4th septum secundum 30s takes out horn from melt, intermittently 30s finishes applying of low frequency stirring magnetic field and high-energy ultrasonic, and reaction finishes the back cooling; refining; skim, add the anti-oxidation of insulating covering agent protection simultaneously, when melt temperature reaches teeming temperature, pour in the water cooled copper mould of diameter 100mm; obtain the matrix material ingot casting; Composite Melt has good flowability, and the matrix material strand outside surface that makes is bright and clean, dense internal organization; do not have loose; solidified structure defectives such as shrinkage cavity, particle size 0.3 ~ 0.5 μM.

Claims (3)

1. the preparation method of a sub-micron granule strengthening aluminum base composite material, to adjust to reacting initial temperature after molten aluminium or the aluminium alloy melt refining, adding can generate particle reactant mutually with molten aluminium or aluminium alloy melt reaction in and carry out building-up reactions, in synthetic reaction process, apply high-energy ultrasonic and low frequency and stir magnetic field, question response finishes, leave standstill and pour into a mould after reducing to teeming temperature, it is characterized in that: high-energy ultrasonic and low frequency stir magnetic field and apply simultaneously, and the high-energy ultrasonic intermittent type applies.
2. the preparation method of a kind of sub-micron granule strengthening aluminum base composite material as claimed in claim 1 is characterized in that: low frequency stirs magnetic field parameter and is: frequency 3Hz, and electric current 150A, low frequency stir magnetic field and apply in the outside in reaction molten bath; The high-energy ultrasonic parameter is: frequency 20kHz, ultrasound intensity 0.8kW/cm 2~ 1.2kW/cm 2, the mode that high-energy ultrasonic applies is that ultrasonic amplitude transformer is reached 5mm ~ 6mm under the melt liquid level.
3. the preparation method of a kind of sub-micron granule strengthening aluminum base composite material as claimed in claim 1, it is characterized in that: high-energy ultrasonic and low frequency stir that magnetic field applies simultaneously and high-energy ultrasonic intermittent type when applying, the time that applies is 3 ~ 5 minutes, the each application time of high-energy ultrasonic 30~50 seconds, 30~50 seconds intermittent times.
CN 201110047197 2011-02-28 2011-02-28 Preparation method of submicron particle-reinforced aluminum-based composite material Pending CN102134667A (en)

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Cited By (17)

* Cited by examiner, † Cited by third party
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CN102586635A (en) * 2011-12-13 2012-07-18 南昌大学 Preparation method of situ Al2O3-particle reinforced Al-Si-Cu composite material semi-solid slurry
CN102776398A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing magnesium-gadolinium intermediate alloy by using high-intensity ultrasound
CN102776393A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing magnesium praseodymium intermediate alloy by using high intensity ultrasonic
CN102776400A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing aluminum gadolinium intermediate alloy by using high intensity ultrasonic
CN102776392A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing magnesium neodymium intermediate alloy with high-intensity ultrasound
CN102776399A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing magnesium holmium intermediate alloy with high-intensity ultrasound
CN102776394A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing aluminum neodymium intermediate alloy with high-intensity ultrasound
CN102776397A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing magnesium samarium intermediate alloy with high-intensity ultrasound
CN102912161A (en) * 2012-07-17 2013-02-06 南昌大学 Method for preparing aluminum cerium intermediate alloy through high-intensity ultrasound
CN103045911A (en) * 2012-07-17 2013-04-17 南昌大学 Method for preparing aluminum-yttrium intermediate alloy by using high intensity ultrasonic
CN103045882A (en) * 2012-07-17 2013-04-17 南昌大学 Method for preparing aluminium praseodymium intermediate alloy in high-energy ultrasonic mode
CN103540805A (en) * 2012-07-17 2014-01-29 南昌大学 Method for preparing aluminum-holmium intermediate alloy by virtue of high-energy ultrasonic
CN103710560A (en) * 2013-12-23 2014-04-09 江苏大学 Method for continuous preparation of aluminum-base in-situ composite material
CN105234356A (en) * 2015-07-14 2016-01-13 南昌大学 Preparation method for aluminum alloy semi-solid slurry induced and impregnated by modificator
CN111041288A (en) * 2019-12-18 2020-04-21 江苏大学 High-toughness anti-fatigue in-situ aluminum-based composite material and preparation method thereof
CN111809075A (en) * 2020-07-03 2020-10-23 西安石油大学 Ti coating Ti3AlC2Particle reinforced Al-based internal combustion engine piston connecting rod and manufacturing method thereof
CN113999980A (en) * 2021-11-05 2022-02-01 合肥工业大学 Preparation device and preparation method of rare earth magnesium alloy

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CN1676641A (en) * 2005-03-31 2005-10-05 江苏大学 Magnetic chemical reaction in-situ synthesizing method for preparing metal base nano composite material
CN1958816A (en) * 2006-11-29 2007-05-09 吉林大学 Technique for preparing composite material of aluminum based surface enhanced by inner generated grains through powered supresonic method
CN101391290A (en) * 2008-11-05 2009-03-25 江苏大学 Method for synthesizing metal matrix composition using metal reaction under the coupling action of magnetic field and ultrasonic field

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CN1676641A (en) * 2005-03-31 2005-10-05 江苏大学 Magnetic chemical reaction in-situ synthesizing method for preparing metal base nano composite material
CN1958816A (en) * 2006-11-29 2007-05-09 吉林大学 Technique for preparing composite material of aluminum based surface enhanced by inner generated grains through powered supresonic method
CN101391290A (en) * 2008-11-05 2009-03-25 江苏大学 Method for synthesizing metal matrix composition using metal reaction under the coupling action of magnetic field and ultrasonic field

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102586635A (en) * 2011-12-13 2012-07-18 南昌大学 Preparation method of situ Al2O3-particle reinforced Al-Si-Cu composite material semi-solid slurry
CN103045882A (en) * 2012-07-17 2013-04-17 南昌大学 Method for preparing aluminium praseodymium intermediate alloy in high-energy ultrasonic mode
CN103540805A (en) * 2012-07-17 2014-01-29 南昌大学 Method for preparing aluminum-holmium intermediate alloy by virtue of high-energy ultrasonic
CN103045911A (en) * 2012-07-17 2013-04-17 南昌大学 Method for preparing aluminum-yttrium intermediate alloy by using high intensity ultrasonic
CN102776392A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing magnesium neodymium intermediate alloy with high-intensity ultrasound
CN102776399A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing magnesium holmium intermediate alloy with high-intensity ultrasound
CN102776394A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing aluminum neodymium intermediate alloy with high-intensity ultrasound
CN102776397A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing magnesium samarium intermediate alloy with high-intensity ultrasound
CN102912161A (en) * 2012-07-17 2013-02-06 南昌大学 Method for preparing aluminum cerium intermediate alloy through high-intensity ultrasound
CN102776400A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing aluminum gadolinium intermediate alloy by using high intensity ultrasonic
CN102776398A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing magnesium-gadolinium intermediate alloy by using high-intensity ultrasound
CN102776393A (en) * 2012-07-17 2012-11-14 南昌大学 Method for preparing magnesium praseodymium intermediate alloy by using high intensity ultrasonic
CN103710560B (en) * 2013-12-23 2016-01-20 江苏大学 A kind of method of continuous production aluminum-based in-situ composite materials
CN103710560A (en) * 2013-12-23 2014-04-09 江苏大学 Method for continuous preparation of aluminum-base in-situ composite material
CN105234356A (en) * 2015-07-14 2016-01-13 南昌大学 Preparation method for aluminum alloy semi-solid slurry induced and impregnated by modificator
CN105234356B (en) * 2015-07-14 2017-05-03 南昌大学 Preparation method for aluminum alloy semi-solid slurry induced and impregnated by modificator
CN111041288A (en) * 2019-12-18 2020-04-21 江苏大学 High-toughness anti-fatigue in-situ aluminum-based composite material and preparation method thereof
CN111809075A (en) * 2020-07-03 2020-10-23 西安石油大学 Ti coating Ti3AlC2Particle reinforced Al-based internal combustion engine piston connecting rod and manufacturing method thereof
CN113999980A (en) * 2021-11-05 2022-02-01 合肥工业大学 Preparation device and preparation method of rare earth magnesium alloy
CN113999980B (en) * 2021-11-05 2023-09-19 合肥工业大学 Preparation device and preparation method of rare earth magnesium alloy

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Application publication date: 20110727