CN104894418A - In-situ synthesized spinel whisker reinforced aluminum-based composite foam and preparation method thereof - Google Patents
In-situ synthesized spinel whisker reinforced aluminum-based composite foam and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a method for preparing spinel whisker reinforced aluminum-based composite foam by in-situ synthesis. The method comprises the following steps of preparing Al-Mg powder according to the mass ratio of 7.4-16 to 1; dropping PVA (Polyvinyl Alcohol) solution with the mass fraction of 3 to 5 percent into the Al-Mg powder according to the mass-to-volume ratio of 13-14g to 1-2ml, grinding the mixture and drying the mixture under the air condition to obtain composite powder, then uniformly mixing the composite powder and NaCl particles according to the mass ratio of 0.29 to 1.16 and pressing the mixture at room temperature and the pressure of 300 to 400MPa into bulk materials; raising the temperature of the bulk materials to be 600 to 800DEG C at the temperature rise rate of 5 to 10DEG C/Min under the atmosphere of argon gases, sintering the bulk materials at the above temperature for 1 to 4 hours and then cooling the sintered materials along with the furnace to obtain an Al-Mg composite material bulk; cleaning the Al-Mg composite material bulk. The method disclosed by the invention has the advantages that the process of preparing foamed aluminium is simple and controllable, and the porosity is adjustable.
Description
Technical field
The present invention relates to a kind of growth in situ MgAl
2o
4the crystal whisker reinforced aluminium-based composite foam of spinel and technology of preparing thereof, be mainly used in the fields such as energy absorption, acoustic absorption, refractory materials.
Technical background
Foamed aluminium take aluminum or aluminum alloy as skeleton, containing the three-dimensional porous metallic substance of a large amount of hilum, owing to having low density, unique surface effects, volume effect, excellent mechanics, electricity, heat and acoustical behavior, for light structure, energy absorption and heat management provide huge potential.
Foam materials energy absorption, shows as and produce large strain under compared with low compressive stress level.This is because it is made up of aluminum alloy framework and a large amount of pore, organize extremely uneven, strain seriously lags behind stress, there is large-scale platform area, thus have good energy absorption capability and larger S. E. A. in compressive stress strain curve.But foamed aluminium is lower due to its plateau stress in actual applications, is also still subject to some restrictions at energy-absorbing and carrying application aspect.
At present, owing to adding some brittle ceramic wild phases outside, such as: Al
2o
3, after SiC and staple fibre, compensate for foam compresses characteristic and energy absorption characteristics to a certain extent, make it be widely used in automobile, transportation by railroad and aerospace field.The preparation of ceramic-phase reinforced body/aluminum-matrix composite foam mainly comprises the methods such as direct foaming, powder metallurgic method, interpolation pore-forming material.Direct foaming owing to having good shaping characteristic and with low cost, thus is widely used in industrial production, but due to the reunion of ceramic phase and surface reaction too much between wild phase and matrix, is therefore very restricted in practical application; Powder metallurgic method due to technique relative complex, and is almost physical contact between ceramic phase and basal body interface, and its wetting property is greatly affected.Above because outer addition makes wild phase skewness in the base, the defects such as interracial contact difference can make its stress-strain(ed) curve in foamed composite compression process obviously fluctuate, and have a significant impact its carrying and energy-absorbing stability.Thus realize ceramic phase in the base dispersed, and keep good interracial contact with matrix, the mechanical property simultaneously improving foam materials is problem demanding prompt solution all the time.
Summary of the invention
The object of the present invention is to provide a kind of fabricated in situ MgAl
2o
4the method of spinel whisker reinforcement foamed aluminium.The method effectively can overcome ceramic phase skewness in the base in outer addition, contacts the defects such as difference with basal body interface.
For achieving the above object, the present invention is realized by the following technical programs,
A method for the crystal whisker reinforced aluminium-based composite foam of fabricated in situ spinel, comprises the following steps:
(1) Al-Mg powder is prepared according to the mass ratio of 7.4 ~ 16:1;
(2) Al-Mg matrix material block is prepared:
Be instill massfraction 3 ~ 5%PVA solution in the Al-Mg powder obtained in step (1) of the proportioning of 13 ~ 14g:1 ~ 2ml according to mass volume ratio, dry under air conditions after grinding, obtained composite powder, then by composite powder and NaCl particle in mass ratio (0.29 ~ 1.16) carry out Homogeneous phase mixing, make block materials in room temperature and 300 ~ 400MPa pressure; Under an argon atmosphere, sinter 1 ~ 4 hour at block materials is warming up to 600 ~ 800 DEG C with temperature rise rate 5 DEG C/min ~ 10 DEG C/min, furnace cooling afterwards, makes Al-Mg matrix material block;
(3) clean by the Al-Mg matrix material block of preparation in step (2), obtained Al composite foam material.
The present invention has the following advantages: it is simple that the method prepares foamed aluminium process, and process control, adjustable porosity, achieves and grown dispersed MgAl at Al matrix situ
2o
4spinel whisker.And this MgAl
2o
4the foamed aluminium of spinel whisker reinforcement, its compression performance is higher than the foamed aluminium that other ceramic phases strengthen.
Accompanying drawing explanation
Fig. 1 is that ball milling obtains homodisperse Al-Mg powder stereoscan photograph after 10 hours.
The foamed aluminium abscess scanning electron microscope (SEM) photograph of Fig. 2 obtained by embodiment 3.
The foamed aluminium hole wall equally distributed MgAl of Fig. 3 obtained by embodiment 3
2o
4spinel whisker stereoscan photograph.
Fig. 4 is MgAl
2o
4the stereoscan photograph of the hexagon end face of spinel whisker rule.
The foamed aluminium compression performance curve of Fig. 5 obtained by embodiment 3.
Embodiment
Fabricated in situ ceramic phase strengthens composite foam method as a kind of new method, can overcome wild phase for a long time dispersed poor in the base, the problem such as interracial contact difference between wild phase and matrix.Relative to other particles or fibrous ceramic phase, MgAl
2o
4spinel whisker be a kind of under manual control condition with a kind of 1-dimention nano fiber of single crystal form growth, not containing the defect existed in usual material, its intensity is close to the theoretical value of perfect cystal.It has lower thermal conductivity, low thermal coefficient of expansion, low specific inductivity and high resistivity on the one hand, simultaneously MgAl
2o
4spinel whisker has the advantage such as high strength, high-melting-point; On the other hand, MgAl
2o
4spinel and Al have cubic structure simultaneously, and MgAl
2o
4in spinel unit cell, oxygen anion sublattice lattice parameter is close with face-centered cubic Al unit cell lattice parameter, thus improves MgAl
2o
4spinel and Al matrix form the possibility of low combination energy in any direction.Therefore it is a kind of desirable reinforcement material.The present invention adopts interpolation pore-forming material method to prepare MgAl
2o
4the aluminum-base composite foam of spinel whisker reinforcement, MgAl in the foamed aluminium of preparation
2o
4spinel whisker is evenly distributed, and whisker is combined well with basal body interface.Relative to other reinforcement materials, by fabricated in situ MgAl in foamed aluminium
2o
4spinel whisker improves its mechanical property by the distortion of existence restriction hole wall in compression of whisker on the one hand, is improved the stability of structure in its compression process on the other hand by whisker.
Generally, fabricated in situ MgAl of the present invention
2o
4the method of the crystal whisker reinforced aluminium-based composite foam of spinel, comprises the following steps:
(1) mechanical ball milling Al-Mg powder
Al, Mg powder quality ratio (7.5 ~ 16), 2 ~ 2.4g boric acid and 0.05 ~ 0.2g stearic acid are placed in ball grinder, carry out mechanical ball milling 9 hours ~ 11 hours with 600 revs/min ~ 800 revs/min, obtained homodisperse Al-Mg powder.
(4) Al-Mg matrix material block is prepared
Instillation 1 ~ 2ml massfraction 3 ~ 5%PVA (polyvinyl alcohol) solution in homodisperse Al-Mg powder obtained in step (1), after grinding under air conditions dry 0.5 ~ 1 hour, then by composite powder and 200-1000um size NaCl particle in mass ratio (0.29 ~ 1.16) carry out Homogeneous phase mixing, make block materials in room temperature and 300 ~ 400MPa pressure.Under an argon atmosphere, 1 ~ 4 hour is sintered at block is warming up to 600 ~ 800 DEG C with temperature rise rate 5 DEG C/min ~ 10 DEG C/min, furnace cooling afterwards.
(5) Al composite foam material is prepared
The Al-Mg matrix material block of preparation in step (2) being spent ionized water 60 DEG C ~ 90 DEG C Water Under baths 12 ~ 24 hours, simultaneously in order to remove NaCl particle fast, changing water every 5 hours.Under 60 DEG C of conditions dry 2 hours subsequently.
Further illustrate the present invention below in conjunction with embodiment, these embodiments, only for illustration of the present invention, do not limit the present invention.
Embodiment 1
Get 11.6gAl powder, 1.56gMg powder, 2.4g boric acid and 0.1g stearic acid with the rotating speed mechanical ball milling 11 hours of 600 revs/min, get powder 6.36g after ball milling, and add 1.5ml massfraction 4%PVA, after grinding dry 1 hour in atmosphere.After being mixed with 8.18gNaCl by powder after grinding, make block materials at room temperature 300MPa pressure.Then in Ar atmosphere with 10 DEG C/min of ramp to 600 DEG C, and be incubated 1 hour.After cooling to room temperature with the furnace, sintering block is placed in 80 DEG C of Water Unders and bathes 24 hours, thus obtain the aluminum-base composite foam of 60% porosity.
Embodiment 2
Get 11.6gAl powder, 1.56gMg powder, 2.4g boric acid and 0.1g stearic acid with the rotating speed mechanical ball milling 11 hours of 750 revs/min, get powder 6.36g after ball milling, and add 1.5ml massfraction 4%PVA, after grinding dry 1 hour in atmosphere.After being mixed with 8.18gNaCl by powder after grinding, make block materials at room temperature 300MPa pressure.Then in Ar atmosphere with 10 DEG C/min of ramp to 600 DEG C, and be incubated 1 hour.After cooling to room temperature with the furnace, sintering block is placed in 80 DEG C of Water Unders and bathes 24 hours, thus obtain the aluminum-base composite foam of 60% porosity.
Embodiment 3
Get 11.6gAl powder, 1.56gMg powder, 2.4g boric acid and 0.1g stearic acid with the rotating speed mechanical ball milling 10 hours of 750 revs/min, get powder 6.36g after ball milling, and add 1.5ml massfraction 4%PVA, after grinding dry 1 hour in atmosphere.After being mixed with 8.18gNaCl by powder after grinding, make block materials at room temperature 300MPa pressure.Then in Ar atmosphere with 10 DEG C/min of ramp to 600 DEG C, and be incubated 1 hour.After cooling to room temperature with the furnace, sintering block is placed in 80 DEG C of Water Unders and bathes 24 hours, thus obtain the aluminum-base composite foam of 60% porosity.
Embodiment 4
Get 11.6gAl powder, 1.56gMg powder, 2.4g boric acid and 0.1g stearic acid with the rotating speed mechanical ball milling 10 hours of 750 revs/min, get powder 6.36g after ball milling, and add 1.5ml massfraction 4%PVA, after grinding dry 1 hour in atmosphere.After being mixed with 8.18gNaCl by powder after grinding, make block materials at room temperature 300MPa pressure.Then in Ar atmosphere with 10 DEG C/min of ramp to 800 DEG C, and be incubated 1 hour.After cooling to room temperature with the furnace, sintering block is placed in 80 DEG C of Water Unders and bathes 24 hours, thus obtain the aluminum-base composite foam of 60% porosity.
Embodiment 5
Get 11.6gAl powder, 1.56gMg powder, 2.4g boric acid and 0.1g stearic acid with the rotating speed mechanical ball milling 10 hours of 750 revs/min, get powder 6.36g after ball milling, and add 1.5ml massfraction 4%PVA, after grinding dry 1 hour in atmosphere.After being mixed with 8.18gNaCl by powder after grinding, make block materials at room temperature 400MPa pressure.Then in Ar atmosphere with 10 DEG C/min of ramp to 800 DEG C, and be incubated 1 hour.After cooling to room temperature with the furnace, sintering block is placed in 80 DEG C of Water Unders and bathes 24 hours, thus obtain the aluminum-base composite foam of 60% porosity.
Embodiment 6
Get 11.6gAl powder, 1.56gMg powder, 2.4g boric acid and 0.1g stearic acid with the rotating speed mechanical ball milling 10 hours of 750 revs/min, get powder 3.17g after ball milling, and add 1.5ml massfraction 4%PVA, after grinding dry 1 hour in atmosphere.After being mixed with 10.9gNaCl by powder after grinding, make block materials at room temperature 400MPa pressure.Then in Ar atmosphere with 10 DEG C/min of ramp to 800 DEG C, and be incubated 1 hour.After cooling to room temperature with the furnace, sintering block is placed in 80 DEG C of Water Unders and bathes 24 hours, thus obtain the aluminum-base composite foam of 80% porosity.
Embodiment 7
Get 12.38gAl powder, 0.78gMg powder, 2.4g boric acid and 0.1g stearic acid with the rotating speed mechanical ball milling 10 hours of 750 revs/min, get powder 6.36g after ball milling, and add 1.5ml massfraction 4%PVA, after grinding dry 1 hour in atmosphere.After being mixed with 8.18gNaCl by powder after grinding, make block materials at room temperature 400MPa pressure.Then in Ar atmosphere with 10 DEG C/min of ramp to 800 DEG C, and be incubated 1 hour.After cooling to room temperature with the furnace, sintering block is placed in 80 DEG C of Water Unders and bathes 24 hours, thus obtain the aluminum-base composite foam of 60% porosity.
Embodiment 8
Get 11.6gAl powder, 1.56gMg powder, 2.4g boric acid and 0.1g stearic acid with the rotating speed mechanical ball milling 10 hours of 750 revs/min, get powder 6.36g after ball milling, and add 1.5ml massfraction 4%PVA, after grinding dry 1 hour in atmosphere.After being mixed with 8.18gNaCl by powder after grinding, make block materials at room temperature 400MPa pressure.Then in Ar atmosphere with 10 DEG C/min of ramp to 800 DEG C, and be incubated 3 hours.After cooling to room temperature with the furnace, sintering block is placed in 80 DEG C of Water Unders and bathes 24 hours, thus obtain the aluminum-base composite foam of 60% porosity.
Summarized by above-mentioned case study on implementation, be prepared according to technique shown in claims, can MgAl be prepared
2o
4spinel whisker reinforcement foamed aluminium, and there is good mechanical property.
By introducing above by reference to the accompanying drawings, invention has been described, but above-mentioned concrete case study on implementation is only schematically can not limit the present invention according to case study on implementation.The person skilled of this area, according to the present invention or when not departing from present inventive concept, can also carry out diversified change, and these distortion are all within protection of the present invention.
Claims (1)
1. a method for the crystal whisker reinforced aluminium-based composite foam of fabricated in situ spinel, comprises the following steps:
(1) Al-Mg powder is prepared according to the mass ratio of 7.4 ~ 16:1;
(2) Al-Mg matrix material block is prepared:
Be instill massfraction 3 ~ 5%PVA solution in the Al-Mg powder obtained in step (1) of the proportioning of 13 ~ 14g:1 ~ 2ml according to mass volume ratio, dry under air conditions after grinding, obtained composite powder, then by composite powder and NaCl particle in mass ratio (0.29 ~ 1.16) carry out Homogeneous phase mixing, make block materials in room temperature and 300 ~ 400MPa pressure; Under an argon atmosphere, sinter 1 ~ 4 hour at block materials is warming up to 600 ~ 800 DEG C with temperature rise rate 5 DEG C/min ~ 10 DEG C/min, furnace cooling afterwards, makes Al-Mg matrix material block;
(3) clean by the Al-Mg matrix material block of preparation in step (2), obtained Al composite foam material.
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| CN105936988A (en) * | 2016-07-13 | 2016-09-14 | 安徽祈艾特电子科技股份有限公司 | Graphene enhanced aluminum magnesium alloy material for automobile electronic packaging and preparing method thereof |
| CN105936992A (en) * | 2016-07-13 | 2016-09-14 | 蚌埠市时代电子有限公司 | Carbon monofluoride enhanced aluminum magnesium alloy material for automobile electronic packaging and preparing method thereof |
| CN106011549A (en) * | 2016-07-13 | 2016-10-12 | 蚌埠市时代电子有限公司 | Nanometer tungsten carbide enhanced aluminum magnesium alloy material for automobile electronic packaging and preparing method of nanometer tungsten carbide enhanced aluminum magnesium alloy material |
| CN106011553A (en) * | 2016-07-13 | 2016-10-12 | 安徽祈艾特电子科技股份有限公司 | Nanometer aluminum oxide reinforced aluminum magnesium alloy material for automobile electronic packaging and preparation method of nanometer aluminum oxide reinforced aluminum magnesium alloy material |
| CN106011552A (en) * | 2016-07-13 | 2016-10-12 | 安徽祈艾特电子科技股份有限公司 | Nanometer titania reinforced aluminum magnesium alloy material for automobile electronic packaging and preparation method of nanometer titania reinforced aluminum magnesium alloy material |
| CN106011550A (en) * | 2016-07-13 | 2016-10-12 | 蚌埠市时代电子有限公司 | Nanometer zirconia enhanced aluminum magnesium alloy material for automobile electronic packaging and preparing method of nanometer zirconia enhanced aluminum magnesium alloy material |
| CN106011551A (en) * | 2016-07-13 | 2016-10-12 | 蚌埠市时代电子有限公司 | Nanometer yttria doping vario-property aluminum magnesium alloy material for automobile electronic packaging and preparing method of nanometer yttria doping vario-property aluminum magnesium alloy material |
| CN106048323A (en) * | 2016-07-13 | 2016-10-26 | 安徽祈艾特电子科技股份有限公司 | Nanosized silicon nitride reinforced aluminium-magnesium alloy material for automobile electronic packaging and preparation method of alloy material |
| CN106048321A (en) * | 2016-07-13 | 2016-10-26 | 安徽祈艾特电子科技股份有限公司 | Nanosized titanium nitride modified and reinforced aluminium-magnesium alloy material for automobile electronic packaging and preparation method of alloy material |
| CN106048322A (en) * | 2016-07-13 | 2016-10-26 | 安徽祈艾特电子科技股份有限公司 | Mesocarbon microbeads modified aluminium-magnesium alloy material for automobile electronic packaging and preparation method of alloy material |
| CN106048324A (en) * | 2016-07-13 | 2016-10-26 | 安徽祈艾特电子科技股份有限公司 | Carbon nano tube reinforced aluminum-magnesium composite alloy material for automobile electronic packaging and preparation method of alloy material |
| CN106148776A (en) * | 2016-07-13 | 2016-11-23 | 安徽祈艾特电子科技股份有限公司 | A kind of automotive electronics encapsulation strengthens hydronalium and preparation method thereof with nanometer silicon carbide |
| CN106191539A (en) * | 2016-07-13 | 2016-12-07 | 蚌埠市时代电子有限公司 | A kind of automotive electronics encapsulation nano-ceramic powder strengthens hydronalium and preparation method thereof |
| CN106191722A (en) * | 2016-07-13 | 2016-12-07 | 安徽祈艾特电子科技股份有限公司 | A kind of automotive electronics encapsulation carbon nano-fiber strengthens antistatic hydronalium and preparation method thereof |
| CN106191540A (en) * | 2016-07-13 | 2016-12-07 | 安徽祈艾特电子科技股份有限公司 | A kind of automotive electronics encapsulation Nano diamond silicon composite strengthening hydronalium and preparation method thereof |
| CN106245076A (en) * | 2016-08-25 | 2016-12-21 | 山东清大银光金属海绵新材料有限责任公司 | The preparation of double whisker reinforcement sponge structure type nickel cobalt molybdenum evanohm high temperature energy-absorbing materials |
| CN110436959A (en) * | 2019-07-31 | 2019-11-12 | 辽宁科技大学 | A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics |
| CN110451994A (en) * | 2019-08-01 | 2019-11-15 | 辽宁科技大学 | A kind of casting material prefabricated part of magnesia firing of magnesium aluminate spinel whisker reinforcement |
| CN114613945A (en) * | 2022-04-02 | 2022-06-10 | 北京师范大学 | Preparation method of lithium ion battery anode |
| CN116715530A (en) * | 2023-06-02 | 2023-09-08 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of spinel carbon material with low thermal expansion rate |
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| CN110436959A (en) * | 2019-07-31 | 2019-11-12 | 辽宁科技大学 | A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics |
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| CN110451994B (en) * | 2019-08-01 | 2022-08-16 | 辽宁科技大学 | Magnesium-based sintered castable prefabricated member reinforced by magnesium aluminate spinel whiskers |
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Application publication date: 20150909 |