CN103695673A - Preparation method of intermetallic compound Al3-M particle reinforced aluminum matrix composite - Google Patents
Preparation method of intermetallic compound Al3-M particle reinforced aluminum matrix composite Download PDFInfo
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Abstract
The invention relates to a preparation method of an intermetallic compound Al3-M particle reinforced aluminum matrix composite and belongs to the technical field of aluminum matrix composite preparation and metal smelting. The invention aims at providing the preparation method of the intermetallic compound Al3-M particle reinforced aluminum matrix composite, and provides the intermetallic compound Al3-M particle reinforced aluminum matrix composite prepared by the method at the same time. The invention adopts the technical scheme that the preparation method of the intermetallic compound Al3-M particle reinforced aluminum matrix composite well solves the problem of no infiltration between an intermetallic compound reinforced particle and molten metal by a stepped method of firstly increasing the magnesium concentration in aluminum melt and adding the intermetallic compound particle.
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 are mainly powder metallurgic method, squeeze casting method, spray deposition, melt infiltration method, in-situ reaction and stirring casting method.Powder metallurgic method is, after enhanced granule and fine pure metal-powder are carried out to mechanically mixing, in mould, to suppress, and then sintering is carried out in heating, makes wild phase and metallic matrix be gathered into one, makes the method for enhanced granule/metal composite.The advantage of powder metallurgic method is mainly that in preparation process, metallic matrix needn't be through the condition of high temperature of fine melt, thereby the problems such as excessive response that occur such as strong oxidation, matrix and enhanced granule interface that can avoid casting to bring, and enhanced granule is evenly distributed in matrix.Powder metallurgic method, to the not restriction of matrix metal kind, can change arbitrarily the proportioning of reinforce and matrix, and the enhanced granule that makes high-volume fractional strengthens metal-base composites.But powder metallurgical technique equipment is complicated, and cost is higher, be difficult for the complex-shaped part of preparation.There is in process of production the danger such as dust-firing, blast, be difficult for 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.During according to casting, metal form difference can be divided into full liquid stirring (one side stirring molten metal, while adding wild phase), Semi-solid Stirring casting (stirring molten metal in semi-solid-state metal melt, add on one side wild phase) and stir founding and make and (in semi-solid-state metal, add wild phase, more than stirring and being warming up to again matrix alloy liquidus temperature after certain hour, and stir again certain hour) three kinds.Stirring casting method equipment is simple, and production efficiency is high, but because wettability between reinforcement and molten aluminium is poor, stirring can not improve the wettability between reinforcement and molten aluminium, therefore bleb is more, size distribution is inhomogeneous, easily forms segregation.
In-situ authigenic reaction particles is synthetic at matrix internal in-situ, basal body interface be combined and interface clean; Can obtain the original position enhanced granule of different sorts, different quantities, the original position of enhanced granule synthetic with casting combine simple process, cost is low, but that the method exists prepared matrix material massfraction is not high.
Research shows, suitable alloying element can be by reducing surface tension and liquid/liquid/solid interface tension force of molten metal, or weaken or suppress the reaction on liquid/liquid/solid interface and improve molten metal to reinforcement wettability of the surface.Theory promotes that with experiment showed, wetting metal belongs to the metal that chemically reactive is stronger mostly.Research is found, for aluminum matrix composite, improving aspect 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 lip-deep oxygen of reinforcement, and its gas blanket of attenuate, improves wettability, reduces enhanced granule or fibre agglomerates trend.
Find by prior art documents, Chinese Patent Application No.: 200910239051.9, open day is 2011.06.29, denomination of invention is: the preparation method of aluminum matrix composite, this patent adopts nano-ceramic particle is joined and is warmed up to liquid state after 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 a kind of intermetallic compound Al for preparing
3the preparation method of-M particle enhanced aluminum-based composite material, adopts substep to improve in advance extraordinary intermetallic compound enhanced granule and the nonwettable problem of molten metal of having solved of method that in molten aluminium, magnesium density adds intermetallic compound particle; The intermetallic compound Al that adopts the method to prepare is provided simultaneously
3the aluminum matrix composite that-M particle strengthens.
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, to the stearic acid that adds composite powder gross weight 0.1%-0.4% in composite powder, ball milling 50-70h under argon atmospher protection then, ratio of grinding media to material 20:1-40:1, 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 ℃, rear furnace cooling;
(3) by the aluminum alloy melting of 50-80wt% and be superheated to 800-850 ℃, heat preservation for standby use;
(4) by the aluminum alloy melting of remaining 20-50wt% to semi-solid state and add pure magnesium, then under argon atmospher protection, the composite powder that accounts for aluminium alloy total mass 1-3% is added in semi-solid aluminium alloy melt, limit edged stirs, and stirs altogether 20-30min; The described amount of adding pure magnesium is two times of the required magnesium name content of whole aluminium alloys;
(5) the overheated aluminium alloy melt of step (3) is punched in the semi-solid aluminium alloy melt of step 4, adjusts temperature to teeming temperature 690-710 ℃, through casting, obtain intermetallic compound Al
3the aluminum matrix composite that-M particle strengthens.
As preferably, described step (3) melts and is superheated to the 55-70% that the aluminium alloy of 800-850 ℃ accounts for 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 of more optimizing is: described step (3) melts and is superheated to the 63-68% that the aluminium alloy of 800-850 ℃ accounts for 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 that method of the present invention is selected is a kind of 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 that described step (4) is added after pure magnesium directly adds composite powder in smelting furnace, powder to be composite is evenly distributed in semi-solid aluminium alloy melt completely, then the overheated aluminium alloy melt of step (3) is poured in smelting furnace, then adjust temperature, pouring cast part;
Method two: described step (4) is added semi-solid aluminium alloy melt after pure magnesium and moved to and add composite powder in tundish again, powder to be composite is evenly distributed in semi-solid aluminium alloy melt completely, then the overheated aluminium alloy melt of 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 μ m, can hinder dislocation motion effectively, plays strengthening effect; And Al
3-M particle and basal body interface are clean, in conjunction with good, can play the effect of transmitted load, and the mechanical property of matrix material is better.
Compared with prior art the present invention has following beneficial effect.
Because particle size is very little time, as enhanced granule of the present invention is of a size of 100nm ~ 1 μ m, surface can increase, more easily reunion.Method of the present invention is first added magnesium in part semi-solid melt, increase the concentration of magnesium, reduce smelt surface tension, make enhanced granule more easily enter melt, at the intermetallic compound particle of preparing high-volume fractional, strengthen aspect metal-base composites, there is very large advantage, solved intermetallic compound enhanced granule add difficultly disperse, with the nonwettable problem of molten metal, simplified nano-scale additive technique, significantly improved intermetallic compound-metal-base composites productive labor condition, reduce cost of manufacture, improved production efficiency.
Adopt method of the present invention can change more neatly the proportioning of intermetallic compound and matrix, make the Al of higher volume fraction
3-M intermetallic compound-metal-base composites, and improved 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 are clean, in conjunction with good, can play the effect of transmitted load; The size of enhanced granule, at submicron order, can hinder dislocation motion effectively, plays strengthening effect.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
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, to the stearic acid that adds composite powder gross weight 0.2% in composite powder, ball milling 60h under argon atmospher protection then, ratio of grinding media to material 20:1, rotational speed of ball-mill 300r/min;
(2) composite powder that ball milling is good dries 4h, rear furnace cooling at 130 ℃ of vacuum drying ovens;
(3) by the aluminum alloy melting of 66wt% and be superheated to 800 ℃, heat preservation for standby use;
(4) by the aluminum alloy melting of remaining 34wt% to semi-solid state and add pure magnesium, then under argon atmospher protection, the composite powder of aluminium alloy total mass 2.5% is added in semi-solid aluminium alloy melt, limit edged stirs, and stirs altogether 25min; The described amount of adding pure magnesium is two times of the required magnesium name content of whole aluminium alloys;
(5) the overheated aluminium alloy melt of step (3) is punched in the semi-solid aluminium alloy melt of step 4, adjusts temperature to 700 ℃ of teeming temperatures, through casting, obtain intermetallic compound Al
3the aluminum matrix composite that-Ti particle strengthens.
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, to the stearic acid that adds composite powder gross weight 0.1% in composite powder, ball milling 65h under argon atmospher protection then, ratio of grinding media to material 30:1, rotational speed of ball-mill 500r/min;
(2) composite powder that ball milling is good dries 5h, rear furnace cooling at 100 ℃ of vacuum drying ovens;
(3) by the aluminum alloy melting of 68wt% and be superheated to 830 ℃, heat preservation for standby use;
(4) by the aluminum alloy melting of remaining 32wt% to semi-solid state and add pure magnesium, then under argon atmospher protection, the composite powder of aluminium alloy total mass 3% is added in semi-solid aluminium alloy melt, limit edged stirs, and stirs altogether 28min; The described amount of adding pure magnesium is two times of the required magnesium name content of whole aluminium alloys;
(5) the overheated aluminium alloy melt of step (3) is punched in the semi-solid aluminium alloy melt of step 4, adjusts temperature to 690 ℃ of teeming temperatures, through casting, obtain intermetallic compound Al
3the aluminum matrix composite that-Ti particle strengthens.
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, to the stearic acid that adds composite powder gross weight 0.2% in composite powder, ball milling 70h under argon atmospher protection then, ratio of grinding media to material 20:1, rotational speed of ball-mill 400r/min;
(2) composite powder that ball milling is good dries 4.5h, rear furnace cooling at 120 ℃ of vacuum drying ovens;
(3) by the aluminum alloy melting of 63wt% and be superheated to 820 ℃, heat preservation for standby use;
(4) by the aluminum alloy melting of remaining 37wt% to semi-solid state and add pure magnesium, then under argon atmospher protection, the composite powder of aluminium alloy total mass 2.5% is added in semi-solid aluminium alloy melt, limit edged stirs, and stirs altogether 24min; The described amount of adding pure magnesium is two times of the required magnesium name content of whole aluminium alloys;
(5) the overheated aluminium alloy melt of step (3) is punched in the semi-solid aluminium alloy melt of step 4, adjusts temperature to 700 ℃ of teeming temperatures, through casting, obtain intermetallic compound Al
3the aluminum matrix composite that-Zr particle strengthens.
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, to the stearic acid that adds composite powder gross weight 0.3% in composite powder, ball milling 50h under argon atmospher protection then, ratio of grinding media to material 40:1, rotational speed of ball-mill 300r/min;
(2) composite powder that ball milling is good dries 3h, rear furnace cooling at 150 ℃ of vacuum drying ovens;
(3) by the aluminum alloy melting of 50wt% and be superheated to 820 ℃, heat preservation for standby use;
(4) by the aluminum alloy melting of remaining 50wt% to semi-solid state and add pure magnesium, then under argon atmospher protection, the composite powder of aluminium alloy total mass 1.5% is added in semi-solid aluminium alloy melt, limit edged stirs, and stirs altogether 30min; The described amount of adding pure magnesium is two times of the required magnesium name content of whole aluminium alloys;
(5) the overheated aluminium alloy melt of step (3) is punched in the semi-solid aluminium alloy melt of step 4, adjusts temperature to 695 ℃ of teeming temperatures, through casting, obtain intermetallic compound Al
3the aluminum matrix composite that-Er particle strengthens.
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, to the stearic acid that adds composite powder gross weight 0.4% in composite powder, ball milling 55h under argon atmospher protection then, ratio of grinding media to material 20:1, rotational speed of ball-mill 600r/min;
(2) composite powder that ball milling is good dries 3.5h, rear furnace cooling at 140 ℃ of vacuum drying ovens;
(3) by the aluminum alloy melting of 80wt% and be superheated to 850 ℃, heat preservation for standby use;
(4) by the aluminum alloy melting of remaining 20wt% to semi-solid state and add pure magnesium, then under argon atmospher protection, the composite powder of aluminium alloy total mass 1% is added in semi-solid aluminium alloy melt, limit edged stirs, and stirs altogether 25min; The described amount of adding pure magnesium is two times of the required magnesium name content of whole aluminium alloys;
(5) the overheated aluminium alloy melt of step (3) is punched in the semi-solid aluminium alloy melt of step 4, adjusts temperature to 710 ℃ of teeming temperatures, through casting, obtain intermetallic compound Al
3the aluminum matrix composite that-Sc particle strengthens.
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, to the stearic acid that adds composite powder gross weight 0.2% in composite powder, ball milling 60h under argon atmospher protection then, ratio of grinding media to material 30:1, rotational speed of ball-mill 500r/min;
(2) composite powder that ball milling is good dries 5h, rear furnace cooling at 120 ℃ of vacuum drying ovens;
(3) by the aluminum alloy melting of 55wt% and be superheated to 800 ℃, heat preservation for standby use;
(4) by the aluminum alloy melting of remaining 45wt% to semi-solid state and add pure magnesium, then under argon atmospher protection, the composite powder of aluminium alloy total mass 2% is added in semi-solid aluminium alloy melt, limit edged stirs, and stirs altogether 20min; The described amount of adding pure magnesium is two times of the required magnesium name content of whole aluminium alloys;
(5) the overheated aluminium alloy melt of step (3) is punched in the semi-solid aluminium alloy melt of step 4, adjusts temperature to 700 ℃ of teeming temperatures, through casting, obtain intermetallic compound Al
3the aluminum matrix composite that-Fe particle strengthens.
The intermetallic compound Al of above-described embodiment gained
3the performance of the aluminum matrix composite that-Ti particle strengthens 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 think explanation of the present invention can not limit invention, claims have been pointed out scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore,, in the implication suitable with claims of the present invention and any variation in scope, all should think to be included in the scope of claims.
Claims (9)
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, to the stearic acid that adds composite powder gross weight 0.1%-0.4% in composite powder, ball milling 50-70h under argon atmospher protection then, ratio of grinding media to material 20:1-40:1, 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 ℃, rear furnace cooling;
(3) by the aluminum alloy melting of 50-80wt% and be superheated to 800-850 ℃, heat preservation for standby use;
(4) by the aluminum alloy melting of remaining 20-50wt% to semi-solid state and add pure magnesium, then under argon atmospher protection, the composite powder that accounts for aluminium alloy total mass 1-3% is added in semi-solid aluminium alloy melt, limit edged stirs, and stirs altogether 20-30min; The described amount of adding pure magnesium is two times of the required magnesium name content of whole aluminium alloys;
(5) the overheated aluminium alloy melt of step (3) is punched in the semi-solid aluminium alloy melt of step 4, adjusts temperature to teeming temperature 690-710 ℃, through casting, obtain intermetallic compound Al
3the aluminum matrix composite that-M particle strengthens.
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 is superheated to the 55-70% that the aluminium alloy of 800-850 ℃ accounts for 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 is superheated to the 63-68% that the aluminium alloy of 800-850 ℃ accounts for 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: described metal M is a kind of in titanium, zirconium, iron, scandium or erbium.
5. 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%.
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 that described step (4) is added after pure magnesium directly adds composite powder in smelting furnace, powder to be composite is evenly distributed in semi-solid aluminium alloy melt completely, then the overheated aluminium alloy melt of step (3) is poured in smelting furnace, then adjust temperature, pouring cast part.
7. 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: described step (4) is added semi-solid aluminium alloy melt after pure magnesium and moved to and in tundish, add composite powder again, powder to be composite is evenly distributed in semi-solid aluminium alloy melt completely, then the overheated aluminium alloy melt of step (3) is poured in tundish, then adjust temperature, pouring cast part.
8. an intermetallic compound Al
3the aluminum matrix composite that-M particle strengthens, is characterized in that: method according to claim 1 is prepared from.
9. a kind of intermetallic compound Al according to claim 8
3the aluminum matrix composite that-M particle strengthens, is characterized in that: described intermetallic compound Al
3the size of-M particle is at 100nm-1 μ m.
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CN106480341A (en) * | 2016-09-21 | 2017-03-08 | 中北大学 | A kind of method of utilization large plastometric set technique preparation richness Al intermetallic reinforcement prefabricated section |
CN106636708A (en) * | 2016-09-21 | 2017-05-10 | 中北大学 | Method for preparing nano intermetallic compound particles and application of particles |
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CN106480341A (en) * | 2016-09-21 | 2017-03-08 | 中北大学 | A kind of method of utilization large plastometric set technique preparation richness Al intermetallic reinforcement prefabricated section |
CN106636708A (en) * | 2016-09-21 | 2017-05-10 | 中北大学 | Method for preparing nano intermetallic compound particles and application of particles |
CN108060321A (en) * | 2017-12-07 | 2018-05-22 | 中北大学 | A kind of preparation method of graphene reinforced aluminum matrix composites |
CN112853163A (en) * | 2021-01-12 | 2021-05-28 | 山东大学 | High-temperature-resistant aluminum alloy composite material and preparation method thereof |
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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