CN101948978B - Preparation method of Al2O3 nanoparticle reinforced aluminum-based composite material - Google Patents
Preparation method of Al2O3 nanoparticle reinforced aluminum-based composite material Download PDFInfo
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- CN101948978B CN101948978B CN 201010505574 CN201010505574A CN101948978B CN 101948978 B CN101948978 B CN 101948978B CN 201010505574 CN201010505574 CN 201010505574 CN 201010505574 A CN201010505574 A CN 201010505574A CN 101948978 B CN101948978 B CN 101948978B
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 77
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 13
- 229910052593 corundum Inorganic materials 0.000 title abstract 5
- 229910001845 yogo sapphire Inorganic materials 0.000 title abstract 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 69
- 239000002245 particle Substances 0.000 claims abstract description 63
- 229910021538 borax Inorganic materials 0.000 claims abstract description 36
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 18
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 60
- 239000011591 potassium Substances 0.000 claims description 60
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 56
- 239000004411 aluminium Substances 0.000 claims description 35
- 239000011159 matrix material Substances 0.000 claims description 35
- 239000004328 sodium tetraborate Substances 0.000 claims description 35
- 239000000376 reactant Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 12
- 101100400378 Mus musculus Marveld2 gene Proteins 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 52
- 229910052751 metal Inorganic materials 0.000 abstract description 17
- 239000002184 metal Substances 0.000 abstract description 17
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract 2
- 229910020148 K2ZrF6 Inorganic materials 0.000 abstract 1
- 229910004844 Na2B4O7.10H2O Inorganic materials 0.000 abstract 1
- 239000011208 reinforced composite material Substances 0.000 abstract 1
- 230000002787 reinforcement Effects 0.000 abstract 1
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 abstract 1
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 239000000155 melt Substances 0.000 description 24
- 239000011734 sodium Substances 0.000 description 22
- 239000008187 granular material Substances 0.000 description 16
- 238000002156 mixing Methods 0.000 description 15
- 239000000463 material Substances 0.000 description 13
- 238000005266 casting Methods 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 12
- 238000002844 melting Methods 0.000 description 12
- 230000008018 melting Effects 0.000 description 12
- 239000002082 metal nanoparticle Substances 0.000 description 12
- 238000007670 refining Methods 0.000 description 12
- 238000005070 sampling Methods 0.000 description 12
- 239000007787 solid Substances 0.000 description 12
- 239000007858 starting material Substances 0.000 description 12
- 238000005303 weighing Methods 0.000 description 12
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 239000002893 slag Substances 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 229910016569 AlF 3 Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910010038 TiAl Inorganic materials 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- -1 CuO Chemical class 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RNUBFUJXCFSMQP-UHFFFAOYSA-N borol-2-one Chemical compound O=C1B=CC=C1 RNUBFUJXCFSMQP-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- BJZIJOLEWHWTJO-UHFFFAOYSA-H dipotassium;hexafluorozirconium(2-) Chemical compound [F-].[F-].[F-].[F-].[F-].[F-].[K+].[K+].[Zr+4] BJZIJOLEWHWTJO-UHFFFAOYSA-H 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Abstract
The invention provides a preparation method of a Al2O3 nanoparticle reinforced aluminum-based composite material, belonging to the technical field of the aluminum-based composite material. The method uses sodium borate (Na2B4O7.10H2O) type boride and K2ZrF6 type fluoride powder as the reaction mixed salt and adopts the direct reaction of molten metal to directly synthetize the nano-Al2O3 particle reinforced aluminum-based composite material in molten aluminum. The invention mainly has the following advantages: the reaction system can effectively control the growth of Al2O3 particles and ensure that the size of the reinforcement phase is controlled to the nanoscale; and the synthesis temperature of the reaction system is 800-850 DEG C, and the defects of the traditional method which uses oxide to prepare the Al2O3 particle reinforced aluminum-based composite material can be overcome, wherein the defects are that the particles are easy to grow, the size can not be controlled and the reaction temperature is high. In addition, with the increase of the addition amount of the reaction mixed salt in the reaction system, the reinforcing particles have smaller size and more uniform distribution; the interface binding of the particles and the substrate is good, no pollution is caused; and the preparation method is an effective method which is suitable for preparing the high-performance nanoparticle reinforced composite material at a low temperature.
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 new system and method for reacting synthesis of nano alumina particle reinforced aluminum matrix composites.
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, melt direct reaction method is the important method of preparation particle enhanced aluminum-based composite material, and this method is through in melt, adding reactant, forms enhanced granule mutually through reactant with in-situ chemical reaction between aluminum substrate.The advantage that this method prepares particles reiforced metal-base composition be that particle is not contaminated with the aluminum substrate interface, the phase interface wettability is good, the power that combines strong and technological process simple relatively etc., therefore receive the attention of domestic and international research day by day.
The alumina particle reinforced aluminum matrix composites is one type of functional structure matrix material with excellent properties; This is because alumina particle and aluminum substrate have good wetting property and interface bond strength; And particle shape is main with the particle than rounding, and physicochemical property, mechanical property and the high-temperature behavior of improving material had extraordinary effect.Extensively adopt oxide compound (like CuO, TiO in the prior art
2, SiO
2, ZrO
2Deng) synthesize preparation alumina particle reinforced aluminum matrix composites with the molten aluminium reaction, but there is following point in such system:
1, initial reaction temperature is high;
2, the aluminium oxide granule particle size that generates is big;
3, particle agglomeration or skewness;
The problems referred to above all have material impact to the preparation and the performance of matrix material.For example, initial reaction temperature is high, makes heat-up time long; Energy consumption is high; And the quality of material had very seriously influence, and particle size is big, group is bunch inhomogeneous to restrict the key issue that material property improves especially; Size is big or roll into a ball bunch strengthening effect that uneven particle is difficult to play, even causes the degradation of material.
At present relevant for Al
2O
3The patent of nanoparticle-reinforced metal matrix composite material.For example the patent No. is that the Chinese patent of CN200710124776.4 has provided and strengthens body with nano aluminium oxide and mix in addition the method for ultrasonic agitation with molten metal and prepare nano particle and strengthen light metal-based matrix material.Though it is simple that this method has technology, series of advantages such as simple controllable, shortcoming such as nano particle is to get into metallic matrix through the mode that adds, and exists the interface that pollution is arranged, and bonding strength is low.The patent No. is that the Chinese patent of CN200510096088.2 utilizes the redox reaction of MOX and metal powder to prepare nanometer Al
2O
3Strengthen the TiAl based composites, implementation step is: with TiO
2, Nb
2O
5Oxide powder is pressed into prefabricated section with after Ti, Al powder mix through high-energy ball milling, places vacuum oven or under the atmosphere protection condition, at 1200 ℃～1250 ℃ sintering temperatures.Though this method has been prepared nanometer Al through the method for in-situ endogenic
2O
3Particle-reinforced TiAl-based composite material, but exist sintering temperature height (energy consumption high), shortcoming such as density is poor, technology is loaded down with trivial details, the equipment that needs is many.
Therefore; Develop a kind of new reaction system; Adopt melt direct reaction method, preparation alumina particle reinforced aluminum matrix composites makes wild phase aluminium oxide granule particle size be easy to be controlled at nanoscale; And the temperature of reaction of this system is low, to solve that the initial reaction temperature that exists of present employing oxide compound and molten aluminium reaction is high, the aluminium oxide granule particle size is big and key issues such as particle agglomeration, bad dispersibility.
Summary of the invention
The objective of the invention is to invent a kind of can be in new system and method than preparation nano alumina particles reinforced aluminum matrix composites under the low reaction temperatures; Particle phase size so that the reaction system that to solve present employing oxide compound be the master exists is out of control, size distribution is inhomogeneous and the high problem of reaction synthesis temperature, with preparation high-performance, the controlled particle enhanced aluminum-based composite material of volume(tric)fraction.
The objective of the invention is to realize through following technical proposal:
Reaction system selects for use the mixture of other borax class pulvis of technical pure level and potassium fluozirconate class pulvis as reacting salt, and the borax class pulvis of employing can be technical pure level n a
2B
4O
710H
2O, B
2O
3Or H
3BO
3In a kind of or its mixture, the potassium fluozirconate class pulvis that is adopted can be other K of technical pure level
2ZrF
6, K
2TiF
6, K
3AlF
6Or Na
3AlF
6In a kind of or its mixture.Adopt melt direct reaction method in the synthetic preparation of molten aluminium internal reaction nano alumina particles reinforced aluminum matrix composites.Borax class pulvis with the ratio of the weight fraction of potassium fluozirconate class pulvis is in the hybrid reaction salt that adopts: 26～31: 74～69.
System of the present invention adopts melt direct reaction synthesis method, promptly earlier with molten aluminium fusing and controlled temperature at synthesis temperature, reactant directly joined behind the mixing in proportion reacts synthetic in the molten aluminium.The temperature of the molten aluminium when reaction is synthetic is controlled at 800～850 ℃.
Adopting course of reaction principle of the present invention, is example with borax and potassium fluorozirconate, is described as follows:
Can know through the thermodynamics of reactions analysis: following reaction will take place in borax-potassium fluozirconate in molten aluminium:
3(K
2ZrF
6)+13[Al]＝3[Al
3Zr]+4(AlF
3)+6KF(g) (1)
(Na
2B
4O
7)+2[Al
3Zr]＝2(ZrB
2)+2Al
2O
3(P)+(Na
2O)+2[Al] (2)
4(K
2ZrF
6)+4[Al]+2(Na
2O)＝4(K
2NaAlF
6)+2(ZrO
2) (3)
With above-mentioned reaction (1)-(3) combination, the total reaction that can obtain this reaction system is:
9(Na
2B
4O
7)+30(K
2ZrF
6)+60[Al]＝
12(ZrO
2)+18(ZrB
2)+13Al
2O
3(P)+18(K
2NaAlF
6)+16(AlF
3)+24KF
(g)(4)
Confirm that through reacted residue being carried out XRD material is K in the slag
2NaAlF
6, ZrB
2, AlF
3, ZrO
2Deng, the XRD figure spectrum of slag is seen Fig. 1, this is slagging because these reactants are easy to reunite, and realizes that the slag gold separates, and Al
2O
3The wettability of particle in aluminium liquid is good; Staying becomes the particle wild phase in the metal melt, Fig. 2 is the transmission electron microscope picture and the SAD collection of illustrative plates of composite as-cast tissue, and Fig. 3 is the XRD figure of matrix material; The result confirms that the particle wild phase in the matrix material is single nano alumina particles.
Potassium fluozirconate (K among the present invention
2ZrF
6) action principle of type fluorochemical is: potassium fluozirconate (K
2ZrF
6) type fluorochemical can generate KF-K with aluminium liquid
3AlF
6(Na
3AlF
6Or K
2NaAlF
6)-AlF
3One type of low-temperature aluminum electrolysis plastome; The characteristics of this type electrolyte system are; Aluminum oxide solubleness therein is very big, and 850 ℃ can reach 9-10wt.%, and the reduction of solubility with temperature and reducing; With the reducing and reduce of KF content, thus the formation mechanism of nano aluminium oxide may be interpreted as react-dissolve-separate out mechanism.In addition, potassium fluozirconate character is active, can be used as tensio-active agent, has increased the activity of each reactant in the reaction, has promptly realized catalytic reaction and the purpose that reduces temperature of reaction.Simultaneously, add K
2ZrF
6Can strengthen the flowability of melt, help improving the dispersion effect that mixes and improve reaction product of reacting salt and molten aluminium, thereby make the tiny dispersion of particle.Fig. 4 has provided the DSC curve of aluminium-borax (Al-B line among the figure), aluminium-borax-potassium fluozirconate (Al-B-Zr line among the figure) two kinds of systems; Can know; Adding potassium fluozirconate can make initial reaction temperature be reduced to about 800 ℃ by about 950 ℃; Corresponding exothermic peak is reduced to about 833 ℃ by about 1016 ℃, explains that adding potassium fluozirconate reduces the initial reaction temperature of reaction system, reaches the purpose that reduces the reaction synthesis temperature.
Compared with prior art the present invention has the following advantages and effect:
1) the present invention adopts borax class boride-potassium fluozirconate class fluorochemical as reaction system; Replacing traditional is main reaction system with the oxide compound; Borolon particle phase size is tiny, can be controlled in nanoscale, has realized the preparation of aluminum oxide nanoparticle reinforced aluminum matrix composites;
2) the alumina particle reinforced aluminum matrix composites of the present invention's preparation, not only particle is tiny, and the particulate distributing homogeneity is good, and this is owing to the peculiar dissolving of multiple intermediate product that adding potassium fluozirconate class fluorochemical is generated, separates out effect;
3) starting temperature of the present invention reaction is low, about 800 ℃, so the temperature of system can be controlled at 800～850 ℃, lower than the synthesis temperature of traditional method, have energy-conservation, improve reaction efficiency and improve multiple beneficial purposes such as quality of materials.
Description of drawings
Fig. 1 is the XRD figure spectrum of slag, to confirm the product in the slag;
Fig. 2 is metal-like transmission electron microscope picture (a) and SAD collection of illustrative plates (b);
Fig. 3 is metalloid XRD figure;
Fig. 4 is the DSC curve of aluminium-borax (Al-B line among the figure), two kinds of systems of aluminium-borax-potassium fluozirconate (Al-B-Zr line among the figure);
Fig. 5 is SEM figure (a) embodiment 1 that embodiment obtains matrix material, and (b) embodiment 2, and (c) embodiment 3;
Fig. 6 is the matrix material SEM figure that embodiment 4 obtains.
Embodiment
Below in conjunction with embodiment the present invention is done further elaboration.Embodiment only is used to explain the present invention, rather than limits the present invention by any way.
Embodiment 1:
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: purity is 98% industrial borax (Na
2B
4O
710H
2O) pulvis and potassium fluozirconate (K
2ZrF
6) pulvis;
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 850 ℃.Agents useful for same borax and potassium fluozirconate all 200 ℃ of oven dry down, grind to form fine powder (granularity is less than 100 μ m), and for use after the weighing, the weight of adding is borax 2Kg, potassium fluozirconate 4.9Kg (weight ratio of borax and potassium fluozirconate 29: 71).
(2): reaction is synthetic:
Behind 850 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
The solidified structure Electronic Speculum figure of material sees Fig. 5 (a).
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: purity is 99.8% industrial borax (Na
2B
4O
710H
2O) pulvis and potassium fluozirconate (K
2ZrF
6) pulvis;
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 830 ℃.Agents useful for same borax and potassium fluozirconate all 200 ℃ of oven dry down, grind to form fine powder (granularity is less than 100 μ m), and for use after the weighing, the weight of adding is borax 4.5Kg, potassium fluozirconate 12Kg (weight ratio of borax and potassium fluozirconate 27: 73).
(2): reaction is synthetic:
Behind 830 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
The solidified structure Electronic Speculum figure of material sees Fig. 5 (b).
Embodiment 3
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: purity is 95.1% industrial borax (Na
2B
4O
710H
2O) pulvis and potassium fluozirconate (K
2ZrF
6) pulvis;
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 800 ℃.Agents useful for same borax and potassium fluozirconate all 200 ℃ of oven dry down, grind to form fine powder (granularity is less than 100 μ m), and for use after the weighing, the weight of adding is borax 6.3Kg, potassium fluozirconate 14Kg (weight ratio of borax and potassium fluozirconate 31: 69).
(2): reaction is synthetic:
Behind 800 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
The solidified structure Electronic Speculum figure of material sees Fig. 5 (c).
Embodiment 4:
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: purity is 98% industrial H
3BO
3Pulvis and potassium fluotitanate (K
2TiF
6) pulvis;
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 850 ℃.Agents useful for same H
3BO
3All dry down at 200 ℃ with potassium fluotitanate, grind to form fine powder (granularity is less than 100 μ m), for use after the weighing, the weight of adding is H
3BO
32Kg, potassium fluotitanate 4.9Kg (H
3BO
3With the weight ratio of potassium fluotitanate 29: 71).
(2): reaction is synthetic:
Behind 850 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
The solidified structure Electronic Speculum figure of material sees Fig. 6.
Embodiment 5:
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: purity is 99.8% industrial H
3BO
3Pulvis and potassium fluoroaluminate (K
3AlF
6) pulvis;
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 830 ℃.Agents useful for same H
3BO
3All dry down at 200 ℃ with potassium fluoroaluminate, grind to form fine powder (granularity is less than 100 μ m), for use after the weighing, the weight of adding is H
3BO
34.5Kg, potassium fluoroaluminate 12Kg (H
3BO
3With the weight ratio of potassium fluoroaluminate 27: 73).
(2): reaction is synthetic:
Behind 830 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: purity is 95.1% industrial H
3BO
3Pulvis and sodium fluoroaluminate (Na
3AlF
6) pulvis;
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 800 ℃.Agents useful for same H
3BO
3Pulvis and sodium fluoroaluminate (Na
3AlF
6) all oven dry under 200 ℃ of pulvis, grinding to form fine powder (granularity is less than 100 μ m), for use after the weighing, the weight of adding is H
3BO
3Pulvis 6.3Kg, sodium fluoroaluminate 14Kg (H
3BO
3Pulvis and sodium fluoroaluminate (Na
3AlF
6) weight ratio 31: 69 of pulvis.
(2): reaction is synthetic:
Behind 800 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
Embodiment 7:
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: purity is 98% industrial borax (Na
2B
4O
710H
2O) pulvis and potassium fluotitanate (K
2TiF
6) pulvis;
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 850 ℃.Agents useful for same borax and potassium fluotitanate all 200 ℃ of oven dry down, grind to form fine powder (granularity is less than 100 μ m), and for use after the weighing, the weight of adding is borax 2Kg, potassium fluotitanate 4.9Kg (weight ratio of borax and potassium fluotitanate 29: 71).
(2): reaction is synthetic:
Behind 850 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
Embodiment 8:
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: purity is 98% industrial borax (Na
2B
4O
710H
2O) pulvis and potassium fluoroaluminate (K
3AlF
6) pulvis;
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 850 ℃.Agents useful for same borax and potassium fluoroaluminate all 200 ℃ of oven dry down, grind to form fine powder (granularity is less than 100 μ m), and for use after the weighing, the weight of adding is borax 2Kg, potassium fluoroaluminate 4.9Kg (weight ratio of borax and potassium fluoroaluminate 29: 71).
(2): reaction is synthetic:
Behind 850 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
Embodiment 9:
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: purity is 98% industrial boric anhydride (B
2O
3) pulvis and potassium fluotitanate (K
2TiF
6) pulvis;
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 850 ℃.Agents useful for same boric anhydride and potassium fluotitanate all 200 ℃ of oven dry down, grind to form fine powder (granularity is less than 100 μ m), and for use after the weighing, the weight of adding is boric anhydride 2Kg, potassium fluotitanate 4.9Kg (weight ratio of boric anhydride and potassium fluotitanate 29: 71).
(2): reaction is synthetic:
Behind 850 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
Embodiment 10:
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: purity is 98% industrial boric anhydride (B
2O
3) pulvis and potassium fluoroaluminate (K
3AlF
6) pulvis;
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 850 ℃.Agents useful for same boric anhydride and potassium fluoroaluminate all 200 ℃ of oven dry down, grind to form fine powder (granularity is less than 100 μ m), and for use after the weighing, the weight of adding is boric anhydride 2Kg, potassium fluoroaluminate 4.9Kg (weight ratio of boric anhydride and potassium fluoroaluminate 29: 71).
(2): reaction is synthetic:
Behind 850 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
Embodiment 11:
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: borax class boride is that purity is 98% industrial boric anhydride (B
2O
3) pulvis and borax (Na
2B
4O
710H
2O) mixture, weight proportion are 1: 1; Potassium fluozirconate class fluorochemical is potassium fluotitanate (K
2TiF
6) pulvis, potassium fluoroaluminate (K
3AlF
6) pulvis and potassium fluozirconate (K
2ZrF
6) mixture, weight proportion is 1: 1: 1.
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 850 ℃.Agents useful for same boride and fluorochemical all 200 ℃ of oven dry down, grind to form fine powder (granularity is less than 100 μ m), and be for use after the weighing, and the weight of adding is for mixing boride 2Kg, mixed fluoride thing 4.9Kg (weight ratio of used boride and fluorochemical 29: 71).
(2): reaction is synthetic:
Behind 850 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
Embodiment 12:
Starting material: commercial-purity aluminium, purity 99.8% (massfraction, down together);
Pressed powder: borax class boride is that purity is 98% industrial boric anhydride (B
2O
3) pulvis, borax (Na
2B
4O
710H
2O) and H
3BO
3Mixture, weight proportion is 1: 1: 1; Potassium fluozirconate class fluorochemical is potassium fluotitanate (K
2TiF
6) pulvis, sodium fluoroaluminate (Na
3AlF
6) pulvis and potassium fluozirconate (K
2ZrF
6) mixture, weight proportion is 1: 1: 1.
The preparation process is following:
(1) at first carry out Metal Melting and powder preparing:
Fine aluminium 100Kg melts in electric furnace and is warmed up to 850 ℃.Agents useful for same boride and fluorochemical all 200 ℃ of oven dry down, grind to form fine powder (granularity is less than 100 μ m), and be for use after the weighing, and the weight of adding is for mixing boride 2Kg, mixed fluoride thing 4.9Kg (weight ratio of used boride and fluorochemical 29: 71).
(2): reaction is synthetic:
Behind 850 ℃ of the melt temperatures, carry out initial refining, in melt, be pressed into the solid reactant powder, adopt strong mixing reaction 10 minutes then with bell jar, after melt temperature is reduced to 730 ℃, slagging-off, casting makes the alumina particle reinforced aluminum matrix composites.
Through sampling analysis, the aluminium oxide granule particle size is less than 100 nanometers, the metal nano-particle reinforced composite.
Claims (4)
1. Al
2O
3The preparation method of nano particle reinforced aluminum matrix composites; It is characterized in that: borax class boride is mixed as reacting salt with potassium fluozirconate class fluorochemical pulvis, adopt melt direct reaction method directly synthetic preparation nano alumina particles reinforced aluminum matrix composites in molten aluminium; Described borax class boride is Na
2B
4O
710H
2O, B
2O
3And H
3BO
3In a kind of mixture of or its any weight ratio, potassium fluozirconate class fluorochemical is K
2ZrF
6, K
2TiF
6, K
3AlF
6And Na
3AlF
6In a kind of mixture of or its any weight ratio; Temperature when reaction is synthetic is controlled at 800～850 ℃; Borax class pulvis and potassium fluozirconate class pulvis blended part by weight are: 26～31: 74～69.
2. a kind of Al according to claim 1
2O
3The preparation method of nano particle reinforced aluminum matrix composites is characterized in that: described borax class boride pulvis and potassium fluozirconate class fluorochemical pulvis are the technical pure rank.
3. a kind of Al according to claim 1
2O
3The preparation method of nano particle reinforced aluminum matrix composites is characterized in that: the add-on of mixed reactant is according to Al
2O
3Required Al in the nano particle reinforced aluminum matrix composites
2O
3The volume(tric)fraction of nano particle is confirmed.
4. a kind of Al according to claim 1
2O
3The preparation method of nano particle reinforced aluminum matrix composites is characterized in that: the Al that reaction generates
2O
3Nanometer wild phase particle size is at 20nm～100nm.
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| CN102745704A (en) * | 2012-07-25 | 2012-10-24 | 深圳市新星轻合金材料股份有限公司 | Method for producing zirconium boride and synchronously outputting cryolite |
| CN103710581B (en) * | 2013-12-27 | 2015-11-18 | 江苏大学 | A kind of nanometer Al 2o 3the preparation method of particle enhanced aluminum-based composite material |
| CN103924128B (en) * | 2014-03-26 | 2016-05-11 | 南昌大学 | A kind of preparation method of nano aluminium oxide reinforced aluminum matrix composites |
| CN104451236B (en) * | 2014-11-07 | 2016-12-07 | 江苏大学 | A kind of nanometer ZrB2the in-situ preparation method of particle enhanced aluminum-based composite material |
| 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 |
| CN107012354B (en) * | 2017-04-05 | 2018-12-14 | 江苏大学 | A kind of preparation method of Al-Si9Cu1 particulate reinforced composite |
| CN109385549B (en) * | 2017-08-04 | 2021-02-02 | 中车大同电力机车有限公司 | Method for smelting cast aluminum of pantograph of electric locomotive |
| CN108359830B (en) * | 2018-02-28 | 2019-10-01 | 江苏大学 | Al3Co coats Al2O3Nanoparticle reinforced aluminum-based composite and preparation method thereof |
| CN111850377B (en) * | 2020-06-18 | 2022-03-22 | 江苏大学 | In-situ Al2O3Preparation method of particle reinforced aluminum matrix composite |
| CN114990390B (en) * | 2022-05-26 | 2023-04-07 | 江苏大学 | Preparation method of in-situ synthesized binary nanoparticle reinforced aluminum matrix composite |
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| US5415708A (en) * | 1993-06-02 | 1995-05-16 | Kballoys, Inc. | Aluminum base alloy and method for preparing same |
| CN1876866A (en) * | 2006-07-06 | 2006-12-13 | 上海交通大学 | Hybrid particles reinforced aluminium-based composite material and preparation method thereof |
| CN1995418A (en) * | 2006-12-28 | 2007-07-11 | 上海交通大学 | Preparation method of granule-mixed reinforced aluminium-based composite material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5415708A (en) * | 1993-06-02 | 1995-05-16 | Kballoys, Inc. | Aluminum base alloy and method for preparing same |
| CN1876866A (en) * | 2006-07-06 | 2006-12-13 | 上海交通大学 | Hybrid particles reinforced aluminium-based composite material and preparation method thereof |
| CN1995418A (en) * | 2006-12-28 | 2007-07-11 | 上海交通大学 | Preparation method of granule-mixed reinforced aluminium-based composite material |
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