CN103695673B - A kind of intermetallic compound particle Al 3the preparation method of-M reinforced aluminum matrix composites - Google Patents
A kind of intermetallic compound particle Al 3the preparation method of-M reinforced aluminum matrix composites Download PDFInfo
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Abstract
A kind of intermetallic compound Al of the present invention
3the preparation method of-M particle enhanced aluminum-based composite material, belongs to aluminum matrix composite preparation and Metal Melting processing technique field; Technical problem to be solved is to provide one and prepares intermetallic compound Al
3the preparation method of-M particle enhanced aluminum-based composite material, provides the intermetallic compound Al adopting the method to prepare simultaneously
3the aluminum matrix composite of-M particle reinforce; The technical scheme adopted is: a kind of intermetallic compound Al
3the preparation method of-M particle enhanced aluminum-based composite material, in employing substep leading raising molten aluminium, the method for magnesium density interpolation intermetallic compound particle is extraordinary solves intermetallic compound enhanced granule and the nonwettable problem of molten metal.
Description
Technical field
A kind of intermetallic compound Al of the present invention
3the preparation method of-M particle enhanced aluminum-based composite material, belongs to aluminum matrix composite preparation and Metal Melting processing technique field.
Background technology
At present, the preparation technology of particles reiforced metal-base composition and method mainly powder metallurgic method, squeeze casting method, spray deposition, molten liquid forming, in-situ reaction and stirring casting method.Powder metallurgic method, after enhanced granule and fine pure metal-powder are carried out mechanically mixing, is suppressed in a mold, and then heating sinters, and makes wild phase and metallic matrix be gathered into one, make the method for enhanced granule/metal composite.The advantage of powder metallurgic method is mainly that in preparation process, metallic matrix need not through the condition of high temperature of fine melt, thus casting can be avoided to bring be such as strongly oxidized, there is the problems such as excessive response in matrix and enhanced granule interface, and enhanced granule is evenly distributed in matrix.Powder metallurgic method does not limit matrix metal kind, can change arbitrarily the proportioning of reinforce and matrix, and the enhanced granule of obtained high-volume fractional strengthens metal-base composites.But powder metallurgical technique equipment is complicated, and cost is higher, not easily prepares complex-shaped part.There is the danger such as dust-firing, blast in process of production, not easily large-scale industrial production.Stirring casting method makes by mechanical stirring, enhanced granule to be joined in metal melt, and makes it finely dispersed method in metallic matrix.Full liquid stirring (stirring molten metal on one side can be divided into according to metal form difference during casting, add wild phase), Semi-solid Stirring casting (while stirring molten metal in semi-solid-state metal melt, while add wild phase) and stir founding and make and (in semi-solid-state metal, add wild phase, stir after certain hour and be warming up to more than matrix alloy liquidus temperature again, and stir certain hour again) three kinds.Stirring casting method equipment is simple, and production efficiency is high, but due to wettability between reinforcement and molten aluminium poor, the wettability that stirring can not improve between reinforcement and molten aluminium, therefore bleb is more, size distribution is uneven, easily forms segregation.
In-situ authigenic reaction particles is at intrinsic silicon fabricated in situ, and basal body interface is combined and clean interfaces; Can obtain the In-sltu reinforcement particle of different sorts, different quantities, the fabricated in situ of enhanced granule combines simple process with casting, cost is low, but the method to there is prepared matrix material massfraction not high.
Research shows, suitable alloying element by reducing surface tension and the liquid/liquid/solid interface tension force of molten metal, or weakens or suppresses the reaction on liquid/liquid/solid interface and improve molten metal to reinforcement wettability of the surface.Theoretical and experiment proves, promotes that wetting metal belongs to the stronger metal of chemically reactive mostly.Research finds, for aluminum matrix composite, improving in the wettability of reinforcement and melting matrix and reinforcement being uniformly distributed in melting matrix, magnesium, as a kind of alloying element, has better effect than Ce, La, Zr, Ti, Bi, Pb, Zn, Cu etc.Magnesium is strong tensio-active agent, is also strong reductor, can react with the oxygen on reinforcement surface, and its gas blanket thinning, improves wettability, reduces enhanced granule or fibre agglomerates trend.
Find by prior art documents, Chinese Patent Application No.: 200910239051.9, publication date is 2011.06.29, denomination of invention is: the preparation method of aluminum matrix composite, the employing of this patent is warmed up to liquid state after being joined by nano-ceramic particle and stirring in semi solid aluminum Base Metal melt and obtains liquid mixed slurry, then after adopting supersound process, cast obtains aluminum matrix composite.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, and technical problem to be solved is to provide one and prepares intermetallic compound Al
3the preparation method of-M particle enhanced aluminum-based composite material, in employing substep leading raising molten aluminium, the method for magnesium density interpolation intermetallic compound particle is extraordinary solves intermetallic compound enhanced granule and the nonwettable problem of molten metal; Provide the intermetallic compound Al adopting the method to prepare simultaneously
3the aluminum matrix composite of-M particle reinforce.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of intermetallic compound Al
3the preparation method of-M particle enhanced aluminum-based composite material, comprises the following steps:
(1) by aluminium powder and metal M powder in molar ratio 3:1 be mixed with composite powder, in composite powder, add the stearic acid of composite powder gross weight 0.1%-0.4%, then ball milling 50-70h, ratio of grinding media to material 20:1-40:1 under argon atmospher protection, rotational speed of ball-mill 300-600r/min;
(2) composite powder that ball milling is good dries 3-5h at vacuum drying oven 100-150 DEG C, rear furnace cooling;
(3) aluminum alloy melting of 50-80wt% is superheated to 800-850 DEG C, heat preservation for standby use;
(4) aluminum alloy melting of remaining 20-50wt% is added pure magnesium to semi-solid state, then add in semi-solid aluminium alloy melt by the composite powder accounting for aluminium alloy total mass 1-3% under argon atmospher protection, limit edged stirs, and stirs 20-30min altogether; Described two times of adding the magnesium name content of amount needed for whole aluminium alloy of pure magnesium;
(5) be punched in the semi-solid aluminium alloy melt of step 4 by aluminium alloy melt overheated for step (3), adjustment temperature, to teeming temperature 690-710 DEG C, obtains intermetallic compound Al through casting
3the aluminum matrix composite of-M particle reinforce.
As preferably, described step (3) melts and the aluminium alloy being superheated to 800-850 DEG C accounts for the 55-70% of aluminium alloy total mass; Described step (4) is melted to the 30-45% that semi-solid aluminium alloy accounts for aluminium alloy total mass.
The scheme more optimized is: described step (3) melts and the aluminium alloy being superheated to 800-850 DEG C accounts for the 63-68% of aluminium alloy total mass; Described step (4) is melted to the 32-37% that semi-solid aluminium alloy accounts for aluminium alloy total mass.
The metal M of method selection of the present invention is the one in titanium, zirconium, iron, scandium or erbium.
The aluminium alloy that the present invention adopts is aluminum silicon alloy, and with hypoeutectic aluminum silicon alloy, in preferred described aluminium alloy, the content of Si is 6% < Si < 11%.
Described by Al
3m enhanced granule addition manner can adopt following methods:
Method one: the semi-solid aluminium alloy melt after described step (4) adds pure magnesium directly adds composite powder in smelting furnace, powder to be composite is evenly distributed in semi-solid aluminium alloy melt completely, then aluminium alloy melt overheated for step (3) is poured in smelting furnace, then adjust temperature, pouring cast part;
Method two: the semi-solid aluminium alloy melt after described step (4) adds pure magnesium moves in tundish and adds composite powder again, powder to be composite is evenly distributed in semi-solid aluminium alloy melt completely, then aluminium alloy melt overheated for step (3) is poured in tundish, then adjust temperature, pouring cast part.
Prepared according to the methods of the invention particle enhanced aluminum-based composite material, described intermetallic compound Al
3--the size of M particle, at 100nm-10 μm, effectively can hinder dislocation motion, play strengthening effect; And Al
3totally, in conjunction with good, can play the effect of transmitted load, the mechanical property of matrix material is more excellent for-M particle and basal body interface.
Compared with prior art the present invention has following beneficial effect.
Due to particle size very little time, as enhanced granule of the present invention is of a size of 100nm ~ 1 μm, surface energy increase, more easily reunite.Method of the present invention first adds magnesium in part semi-solid melt, increase the concentration of magnesium, reduce smelt surface tension, enhanced granule is made more easily to enter melt, strengthen in metal-base composites at the intermetallic compound particle preparing high-volume fractional, there is very large advantage, solve intermetallic compound enhanced granule add difficult dispersion, with the nonwettable problem of molten metal, simplify nano-scale additive technique, significantly improve intermetallic compound-metal-base composites productive labor condition, reduce cost of manufacture, improve production efficiency.
Adopt method of the present invention can change the proportioning of intermetallic compound and matrix more neatly, the Al of obtained higher volume fraction
3-M intermetallic compound-metal-base composites, and improve Al
3the degree of scatter of-M intermetallic compound in metallic matrix.
Matrix material prepared by method of the present invention, Al
3-M particle and basal body interface totally, in conjunction with good, can play the effect of transmitted load; The size of enhanced granule, at submicron order, effectively can hinder dislocation motion, play strengthening effect.
Accompanying drawing explanation
Fig. 1 is present invention process schema.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of intermetallic compound Al
3the preparation method of-Ti particle enhanced aluminum-based composite material, comprises the following steps:
(1) by aluminium powder and metal Ti powder in molar ratio 3:1 be mixed with composite powder, in composite powder, add the stearic acid of composite powder gross weight 0.2%, then ball milling 60h, ratio of grinding media to material 20:1 under argon atmospher protection, rotational speed of ball-mill 300r/min;
(2) composite powder that ball milling is good dries 4h at vacuum drying oven 130 DEG C, rear furnace cooling;
(3) aluminum alloy melting of 66wt% is superheated to 800 DEG C, heat preservation for standby use;
(4) aluminum alloy melting of remaining 34wt% is added pure magnesium to semi-solid state, then add in semi-solid aluminium alloy melt by the composite powder of aluminium alloy total mass 2.5% under argon atmospher protection, limit edged stirs, and stirs 25min altogether; Described two times of adding the magnesium name content of amount needed for whole aluminium alloy of pure magnesium;
(5) be punched in the semi-solid aluminium alloy melt of step 4 by aluminium alloy melt overheated for step (3), adjustment temperature, to teeming temperature 700 DEG C, obtains intermetallic compound Al through casting
3the aluminum matrix composite of-Ti particle reinforce.
Embodiment 2
A kind of intermetallic compound Al
3the preparation method of-Ti particle enhanced aluminum-based composite material, comprises the following steps:
(1) by aluminium powder and metal Ti powder in molar ratio 3:1 be mixed with composite powder, in composite powder, add the stearic acid of composite powder gross weight 0.1%, then ball milling 65h, ratio of grinding media to material 30:1 under argon atmospher protection, rotational speed of ball-mill 500r/min;
(2) composite powder that ball milling is good dries 5h at vacuum drying oven 100 DEG C, rear furnace cooling;
(3) aluminum alloy melting of 68wt% is superheated to 830 DEG C, heat preservation for standby use;
(4) aluminum alloy melting of remaining 32wt% is added pure magnesium to semi-solid state, then add in semi-solid aluminium alloy melt by the composite powder of aluminium alloy total mass 3% under argon atmospher protection, limit edged stirs, and stirs 28min altogether; Described two times of adding the magnesium name content of amount needed for whole aluminium alloy of pure magnesium;
(5) be punched in the semi-solid aluminium alloy melt of step 4 by aluminium alloy melt overheated for step (3), adjustment temperature, to teeming temperature 690 DEG C, obtains intermetallic compound Al through casting
3the aluminum matrix composite of-Ti particle reinforce.
Embodiment 3
A kind of intermetallic compound Al
3the preparation method of-Zr particle enhanced aluminum-based composite material, comprises the following steps:
(1) by aluminium powder and metallic Z r powder in molar ratio 3:1 be mixed with composite powder, in composite powder, add the stearic acid of composite powder gross weight 0.2%, then ball milling 70h, ratio of grinding media to material 20:1 under argon atmospher protection, rotational speed of ball-mill 400r/min;
(2) composite powder that ball milling is good dries 4.5h at vacuum drying oven 120 DEG C, rear furnace cooling;
(3) aluminum alloy melting of 63wt% is superheated to 820 DEG C, heat preservation for standby use;
(4) aluminum alloy melting of remaining 37wt% is added pure magnesium to semi-solid state, then add in semi-solid aluminium alloy melt by the composite powder of aluminium alloy total mass 2.5% under argon atmospher protection, limit edged stirs, and stirs 24min altogether; Described two times of adding the magnesium name content of amount needed for whole aluminium alloy of pure magnesium;
(5) be punched in the semi-solid aluminium alloy melt of step 4 by aluminium alloy melt overheated for step (3), adjustment temperature, to teeming temperature 700 DEG C, obtains intermetallic compound Al through casting
3the aluminum matrix composite of-Zr particle reinforce.
Embodiment 4
A kind of intermetallic compound Al
3the preparation method of-Er particle enhanced aluminum-based composite material, comprises the following steps:
(1) by aluminium powder and metal Er powder in molar ratio 3:1 be mixed with composite powder, in composite powder, add the stearic acid of composite powder gross weight 0.3%, then ball milling 50h, ratio of grinding media to material 40:1 under argon atmospher protection, rotational speed of ball-mill 300r/min;
(2) composite powder that ball milling is good dries 3h at vacuum drying oven 150 DEG C, rear furnace cooling;
(3) aluminum alloy melting of 50wt% is superheated to 820 DEG C, heat preservation for standby use;
(4) aluminum alloy melting of remaining 50wt% is added pure magnesium to semi-solid state, then add in semi-solid aluminium alloy melt by the composite powder of aluminium alloy total mass 1.5% under argon atmospher protection, limit edged stirs, and stirs 30min altogether; Described two times of adding the magnesium name content of amount needed for whole aluminium alloy of pure magnesium;
(5) be punched in the semi-solid aluminium alloy melt of step 4 by aluminium alloy melt overheated for step (3), adjustment temperature, to teeming temperature 695 DEG C, obtains intermetallic compound Al through casting
3the aluminum matrix composite of-Er particle reinforce.
Embodiment 5
A kind of intermetallic compound Al
3the preparation method of-Sc particle enhanced aluminum-based composite material, comprises the following steps:
(1) by aluminium powder and metal Sc powder in molar ratio 3:1 be mixed with composite powder, in composite powder, add the stearic acid of composite powder gross weight 0.4%, then ball milling 55h, ratio of grinding media to material 20:1 under argon atmospher protection, rotational speed of ball-mill 600r/min;
(2) composite powder that ball milling is good dries 3.5h at vacuum drying oven 140 DEG C, rear furnace cooling;
(3) aluminum alloy melting of 80wt% is superheated to 850 DEG C, heat preservation for standby use;
(4) aluminum alloy melting of remaining 20wt% is added pure magnesium to semi-solid state, then add in semi-solid aluminium alloy melt by the composite powder of aluminium alloy total mass 1% under argon atmospher protection, limit edged stirs, and stirs 25min altogether; Described two times of adding the magnesium name content of amount needed for whole aluminium alloy of pure magnesium;
(5) be punched in the semi-solid aluminium alloy melt of step 4 by aluminium alloy melt overheated for step (3), adjustment temperature, to teeming temperature 710 DEG C, obtains intermetallic compound Al through casting
3the aluminum matrix composite of-Sc particle reinforce.
Embodiment 6
A kind of intermetallic compound Al
3the preparation method of-Fe particle enhanced aluminum-based composite material, comprises the following steps:
(1) by aluminium powder and metal iron powder in molar ratio 3:1 be mixed with composite powder, in composite powder, add the stearic acid of composite powder gross weight 0.2%, then ball milling 60h, ratio of grinding media to material 30:1 under argon atmospher protection, rotational speed of ball-mill 500r/min;
(2) composite powder that ball milling is good dries 5h at vacuum drying oven 120 DEG C, rear furnace cooling;
(3) aluminum alloy melting of 55wt% is superheated to 800 DEG C, heat preservation for standby use;
(4) aluminum alloy melting of remaining 45wt% is added pure magnesium to semi-solid state, then add in semi-solid aluminium alloy melt by the composite powder of aluminium alloy total mass 2% under argon atmospher protection, limit edged stirs, and stirs 20min altogether; Described two times of adding the magnesium name content of amount needed for whole aluminium alloy of pure magnesium;
(5) be punched in the semi-solid aluminium alloy melt of step 4 by aluminium alloy melt overheated for step (3), adjustment temperature, to teeming temperature 700 DEG C, obtains intermetallic compound Al through casting
3the aluminum matrix composite of-Fe particle reinforce.
The intermetallic compound Al of above-described embodiment gained
3the performance of the aluminum matrix composite of-Ti particle reinforce is in table 1.
The present invention can summarize with other the specific form without prejudice to spirit of the present invention or principal character.Therefore, no matter from that, above-mentioned embodiment of the present invention all can only be thought explanation of the present invention and can not limit invention, claims indicate scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, any change in the implication suitable with claims of the present invention and scope, all should think to be included in the scope of claims.
Claims (8)
1. an intermetallic compound Al
3the preparation method of-M particle enhanced aluminum-based composite material, is characterized in that comprising the following steps:
(1) by aluminium powder and metal M powder in molar ratio 3:1 be mixed with composite powder, in composite powder, add the stearic acid of composite powder gross weight 0.1%-0.4%, then ball milling 50-70h, ratio of grinding media to material 20:1-40:1 under argon atmospher protection, rotational speed of ball-mill 300-600r/min; Described metal M is the one in titanium, zirconium, iron, scandium or erbium;
(2) composite powder that ball milling is good dries 3-5h at vacuum drying oven 100-150 DEG C, rear furnace cooling;
(3) aluminum alloy melting of 50-80wt% is superheated to 800-850 DEG C, heat preservation for standby use;
(4) aluminum alloy melting of remaining 20-50wt% is added pure magnesium to semi-solid state, then add in semi-solid aluminium alloy melt by the composite powder accounting for aluminium alloy total mass 1-3% under argon atmospher protection, limit edged stirs, and stirs 20-30min altogether; Described two times of adding the magnesium name content of amount needed for whole aluminium alloy of pure magnesium;
(5) be punched in the semi-solid aluminium alloy melt of step 4 by aluminium alloy melt overheated for step (3), adjustment temperature, to teeming temperature 690-710 DEG C, obtains intermetallic compound Al through casting
3the aluminum matrix composite of-M particle reinforce.
2. a kind of intermetallic compound Al according to claim 1
3the preparation method of-M particle enhanced aluminum-based composite material, is characterized in that: described step (3) melts and the aluminium alloy being superheated to 800-850 DEG C accounts for the 55-70% of aluminium alloy total mass; Described step (4) is melted to the 30-45% that semi-solid aluminium alloy accounts for aluminium alloy total mass.
3. a kind of intermetallic compound Al according to claim 2
3the preparation method of-M particle enhanced aluminum-based composite material, is characterized in that: described step (3) melts and the aluminium alloy being superheated to 800-850 DEG C accounts for the 63-68% of aluminium alloy total mass; Described step (4) is melted to the 32-37% that semi-solid aluminium alloy accounts for aluminium alloy total mass.
4. a kind of intermetallic compound Al according to claim 1 and 2
3the preparation method of-M particle enhanced aluminum-based composite material, is characterized in that: in described aluminium alloy, the content of Si is 6% < Si < 11%.
5. a kind of intermetallic compound Al according to claim 1 and 2
3the preparation method of-M particle enhanced aluminum-based composite material, it is characterized in that: the semi-solid aluminium alloy melt after described step (4) adds pure magnesium directly adds composite powder in smelting furnace, powder to be composite is evenly distributed in semi-solid aluminium alloy melt completely, then aluminium alloy melt overheated for step (3) is poured in smelting furnace, then adjust temperature, pouring cast part.
6. a kind of intermetallic compound Al according to claim 1 and 2
3the preparation method of-M particle enhanced aluminum-based composite material, it is characterized in that: the semi-solid aluminium alloy melt after described step (4) adds pure magnesium moves in tundish and adds composite powder again, powder to be composite is evenly distributed in semi-solid aluminium alloy melt completely, then aluminium alloy melt overheated for step (3) is poured in tundish, then adjust temperature, pouring cast part.
7. an intermetallic compound Al
3the aluminum matrix composite of-M particle reinforce, is characterized in that: method according to claim 1 is prepared from.
8. a kind of intermetallic compound Al according to claim 7
3the aluminum matrix composite of-M particle reinforce, is characterized in that: described intermetallic compound Al
3the size of-M particle is at 100nm-1 μm.
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| CN106480341B (en) * | 2016-09-21 | 2018-04-17 | 中北大学 | A kind of method that rich Al intermetallic reinforcement prefabricated section is prepared using large plastometric set technique |
| CN106636708A (en) * | 2016-09-21 | 2017-05-10 | 中北大学 | Method for preparing nano intermetallic compound particles and application of particles |
| CN108060321B (en) * | 2017-12-07 | 2019-06-11 | 中北大学 | A kind of preparation method of graphene reinforced aluminum matrix composites |
| CN112853163B (en) * | 2021-01-12 | 2021-09-14 | 山东大学 | High-temperature-resistant aluminum alloy composite material and preparation method thereof |
| CN115572883A (en) * | 2022-10-11 | 2023-01-06 | 重庆三航新材料技术研究院有限公司 | Preparation method of SiCp reinforced aluminum-based composite material for stirring casting |
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