CN104046825A - Preparation method of in-situ particle reinforced aluminum-based composite material - Google Patents
Preparation method of in-situ particle reinforced aluminum-based composite material Download PDFInfo
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- CN104046825A CN104046825A CN201410316034.1A CN201410316034A CN104046825A CN 104046825 A CN104046825 A CN 104046825A CN 201410316034 A CN201410316034 A CN 201410316034A CN 104046825 A CN104046825 A CN 104046825A
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Abstract
The invention relates to the technical field of a composite material, and particularly relates to a preparation method of an in-situ particle reinforced aluminum-based composite material. According to the preparation method, an element compound formed by taking ceramic reaction powder without reaction side products as reinforcement particles is formed to replace the traditional villiaumite, and by combining the sintering and wetting of ceramic reaction powder, ultrasonic dispersion and compounding and liquid-state forming, the problems that the ceramic reaction powder of the composite material during the preparation process is not wetted, and difficult to react, and the generated fine reinforcements are massively clustered and the like and can be effectively solved. The preparation method has the advantages of no pollution, high reaction element yield and good reinforcement uniformity, is environmental friendly, the low-cost and massive preparation of large-size composite material members can be realized, and the engineering application of the particle reinforced aluminum-based composite material can be favorably promoted.
Description
Technical field
The present invention relates to technical field of composite materials, specifically a kind of aluminum based composite material enhanced by granules in situ preparation method.
Background technology
Good performances such as the specific tenacity of particle enhanced aluminum-based composite material Yin Qigao, specific modulus, high heat conduction, low bulk and being paid close attention to widely, have huge application potential in fields such as aerospace, Electronic Packaging, the energy and communications and transportation; Wherein compare with additional reinforced particulate, adopt in aluminum matrix composite prepared by in-situ method reinforcement generally more tiny (<2 μ m), strong plasticity to raising matrix material is favourable, simultaneously because reinforcement forming core in matrix is grown up, for thermodynamically stable phase, and realize metallurgical binding with matrix, can significantly improve the high-temperature service performance of matrix material.
Existing technical literature and Review literature investigation are shown, relatively ripe in-situ Al-base composition preparation method is mainly mixing salt reaction method (liquid phase process) (as: patent CN200510028209.X and CN200710036338.2) and powder metallurgic method (solid state process) (as: patent CN200510010038.8 and CN01106345.9) at present; Wherein because the pottery such as oxide compound reaction pulvis and aluminium immersion lubricant nature are poor, cause and react pulvis and be difficult to add in molten aluminium, so liquid phase process is prepared in the process of in-situ Al-base composition common with the villiaumite (as: Al-K good with aluminium liquid phase capacitive
2tiF
6-KBF
4reaction system) for reinforcement particle forms element compound, i.e. mixing salt reaction method; The particle of powder metallurgic method forms element compound and chooses the ceramic pulvis (as: Al-TiO such as the oxide compound of reactionless by product, carbide
2-B
2o
3reaction system); Yet aforesaid method still exists following shortcoming and defect (1) mixed salt method and pollutes large: villiaumite not only can produce a large amount of reaction slags with reacting of aluminium liquid, and the flue gas producing in reaction process is large to human body and equipment harm; (2) powder metallurgic method densification is difficult, cost is high: because reaction system is generally quick thermopositive reaction, the meeting of heat release rapidly in sintering process causes composite inner to produce the defects such as a large amount of cavities, sintered blank also will be passed through secondary deformation (extruding, forging, rolling etc.) and could be obtained fine and close composite element simultaneously, and cost is increased substantially.
Summary of the invention
Object of the present invention is just for the deficiencies in the prior art, by reaction powder sintering infiltrate, ultrasonic dispersion is compound and liquid condition shaping combines, the pottery reaction pulvis of the reactionless by products such as oxide compound, carbide of take is raw material, adopts that liquid phase process is green, efficient, low-cost, original position is prepared particle enhanced aluminum-based composite material.
First the present invention realizes infiltration, the combination of pottery reaction pulvis and aluminium by the sintering of compound powder blank; Then compound powder sintered blank is dropped in aluminium liquid, make sintered blank incorporate aluminium liquid, and promote stirring, the accelerated reaction of melt to carry out disperseing with reinforcement by ultrasonic method; Finally by compounding flux by the method for liquid condition shaping, obtain expeditiously composite element.
The present invention effectively solves in matrix material preparation process that pottery reaction pulvis does not infiltrate, react that difficulty, reaction pulvis utilization ratio are low, the tiny reinforcement that the generates problem such as reunions in a large number, can be pollution-free, low-cost, high-level efficiency, macroblock quantization prepare particle enhanced aluminum-based composite material.
Preparation method of the present invention comprises the following steps:
(1) preparation of compound powder blank: the method for pottery being reacted to pulvis and aluminium powder employing ball milling is evenly mixed and is cold-pressed into base, is then placed in atmosphere or vacuum oven sintering, makes aluminium powder thawing Host range pulvis in pressed compact obtain sintered blank.
(2) ultrasonic dispersion is compound: the fine aluminium as matrix or its alloy are heated to pulvis temperature of reaction insulation, then sintered blank is dropped in molten aluminium, melt is applied to ul-trasonic irradiation simultaneously, by hyperacoustic cavitation, acoustic streaming effect, promote the carrying out of the stirring of melt, the dispersion of pulvis and reaction.
(3) molding component: the Composite Melt obtaining is carried out after refining, slagging-off, degasification and inoculation, adopt the method for liquid condition shaping to obtain composite element.
Described reaction pulvis is ZrO
2ceramic powder, TiO
2ceramic powder, ZrO
2and B
2o
3mixture (mol ratio 1:1), ZrO
2mixture (mol ratio 1:2), TiO with B
2and B
2o
3mixture (mol ratio 1:1), TiO
2mixture (mol ratio 1:2) or TiO with B
2and B
4the mixture of C (mol ratio 3:1); The content of its reaction pulvis is for the pottery reaction pulvis of ball milling and 20 ~ 50vol.% of aluminium powder cumulative volume.
The described pressure of colding pressing that is cold-pressed into base is 300MPa, and the base density of colding pressing is 70% ~ 85%.
Described aluminium powder is identical with matrix composition, a kind of in fine aluminium or its alloy, and the particle diameter of aluminium powder is 2 ~ 50 μ m.
Described ball milling, object is the even mixing of realization response pulvis and reinforcement, conventionally adopts the method for high-energy ball milling, and this technology adopts 1-S lab stirring ball mill, and rotational speed of ball-mill is 426r/min, and ratio of grinding media to material is 20:1, Ball-milling Time 1h.
Described sintering temperature is above 50 ~ 150 ℃ of matrix alloy fusing point, and sintering time is 0.5 ~ 2h.
Described is ultrasonic, and its parameter is velocity of wave 1500m/s, frequency 20kHz, power 500 ~ 1500W, time 10 ~ 30min.
Described refining, slagging-off, degasification and inoculation, object is to remove residual slag, impurity and gas in compounding flux, breeds generation nucleus, finally obtains dense structure, composite element that crystal grain is tiny.
Existing mixed salt method is prepared in-situ Al-base composition, due to ceramic-like reaction pulvis (ZrO such as oxide compound, carbide
2, B
2o
3, TiO
2deng) all there is high-melting-point, and with the feature such as aluminium liquid wetting is poor, therefore, the liquid preparation method of particle enhanced aluminum-based composite material, adopts the villiaumite (as: K that fusing point is low and good with molten aluminium consistency conventionally
2tiF
6+ KBF
4or K
2zrF
6+ KBF
4deng) be the agent of reinforcement particle formation element reaction.Yet villiaumite and molten aluminium react and generate in the process of reinforcement and can produce a large amount of slags and flue gas (KAlF at bath surface
4, K
3alF), large to human body and equipment harm, the fluorine containing corrosion flue gas that especially under high temperature, villiaumite and reaction product volatilization thereof produce makes electric stove wire seriously corroded, causes significantly shorten the work-ing life of electric furnace, is difficult to large-scale promotion application.
Existing powder metallurgic method is prepared aluminum based composite material enhanced by granules in situ, due to mixing and densification that reaction pulvis is solid-state form with aluminium powder form, there is not the problems such as infiltration between reaction pulvis and aluminium liquid, dispersion, so conventionally adopt the pottery reaction pulvis such as oxide compound as the compound of particle forming element, thereby do not have the by products such as slag, the relative mixed salt method of this preparation method has cleaning, free of contamination advantage.But, the production cost of this height of powder metallurgic method, especially in reinforcement particle formation reaction process, the large calorimetric of instantaneous generation is easy to cause cavity, defects i.e.cracks, sintered blank will adopt further hot pressing densification and secondary deformation could obtain fine and close matrix material blank conventionally, finally also to pass through secondary deformation (extruding, forge, rolling etc.) could obtain composite element, cost is increased substantially, and with liquid condition shaping (sand casting, pressure die casting etc.) compare, conventionally can only obtain the member of simple shape, thereby, powder metallurgic method is prepared in-situ particle reinforcement aluminum matrix composite, because there is complicated process of preparation in it, cost is high, be difficult to manufacture the shortcomings such as complex shaped components, also limited its mass-producing application.
The present invention reacts pottery that pulvis sintering infiltrates, ultrasonic dispersion is compound and liquid condition shaping combines, and take oxide compound, carbide reaction pulvis is raw material, adopts that liquid phase process is green, efficient, low cost, macroblock quantization, original position prepare particle enhanced aluminum-based composite material, composite wood is prepared microprocess schematic diagram as shown in Figure 1, by pottery, react near the sintering of pulvis-aluminium powder composite powder base temperature range aluminium fusing point, make in blank aluminium powder melt and with react pulvis and infiltrates acquisition compound sintered compact, then sintered blank is dropped in the aluminium liquid of melting, because making surface in sintered blank, the thawing of aluminium in sintered blank is scattered in melt with the pulvis that reacts of aluminium infiltration, avoid in directly reaction pulvis being added to molten aluminium because powder and aluminium liquid do not infiltrate freely reuniting that (surface energy is high) produce, under ultrasonic effect, react pulvis dispersed and react and generate tiny uniform reinforcement particle with aluminium liquid simultaneously, in refining, slagging-off, after degasification and inoculation, compounding flux is obtained to required composite element by the method for casting.
Compare with traditional mixed salt method, the present invention adopts oxide compound, carbide etc. as reinforcement particle, to form element compound without slag pottery reaction pulvis, in compound preparation process, do not produce slag and volatilization gas, make that the preparation of matrix material has that reaction pulvis utilization ratio is high, low price, high-level efficiency, oligosaprobic environmental protection feature; Sintering by composite powder base solves pottery reaction pulvis and aluminium immersion profit problem difficult, that easily reunite; In preparation process by apply ultrasonication, can further improve the dispersion of dispersion, reaction and the reinforcement that generates of ceramic pulvis; Compare with traditional powder metallurgic method, the present invention adopts liquid method moulding, not only have with low cost, macroblock quantization is produced the composite component of complicated shape in enormous quantities; But also can avoid quick heat release in recombination process to produce cavity, defects i.e.cracks in composite inner.Thereby the present invention can be green, efficient, low-cost, macroblock quantization is prepared aluminum based composite material enhanced by granules in situ and member thereof, is conducive to promote the through engineering approaches application of particle enhanced aluminum-based composite material.
Accompanying drawing explanation
Fig. 1 matrix material of the present invention is prepared microprocess schematic diagram.
Fig. 2 composite material preparation process schema of the present invention.
Compound sintered compact Photomicrograph (ZrO prepared by Fig. 3 the present invention
2and Al).
(Al prepared by Fig. 4 the present invention
3zr+Al
2o
3)/Al microstructure of composite photo.
Embodiment
Below in conjunction with accompanying drawing, embodiment of the present invention is further described: following examples are implemented take technical solution of the present invention under prerequisite; provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.Matrix material is prepared microprocess schematic diagram as shown in Figure 1, the schema of composite material preparation process shown in Fig. 2.
Embodiment 1
With ZrO
2for reaction pulvis original position preparation (Al
3zr+Al
2o
3)/Al matrix material.
By analytical pure ZrO
2powder (30vol.%) and middle particle diameter are that the spherical fine aluminium powder (70vol.%) of 10 μ m is put into 1-S lab ball mill ball milling and prepared compound powder, ball-milling medium is Stainless Steel Ball (diameter 6mm), ratio of grinding media to material is 20:1, rotational speed of ball-mill is 426r/min, Ball-milling Time is 1h, finally prepares ZrO
2the mixed uniformly compound powder powder of powder and aluminium powder; Getting 100g compound powder powder to put into diameter be that the mould of 40mm is cold-pressed into is highly the compound powder pressed compact of 40mm, and the pressure of colding pressing is 300MPa; The base of colding pressing is put into the atmosphere furnace sintering that is connected with argon gas, sintering temperature is 750 ℃, and sintering time is 1h, obtains sintered blank, is illustrated in figure 3 compound sintered compact microstructure picture; The fine aluminium ingot that is 500g by quality is put into crucible oven and is melted and be incubated to 950 ℃, then compound powder sintered blank is put into molten aluminium and applied ultrasonication, power 1500W, ultrasonic 10min, along with the aluminium fusing in the prolongation sintered blank of ultrasonic time, also release reaction pulvis is in aluminium liquid, and the while is impelled ZrO under ultrasonic effect
2rapid dispersion, after being wrapped in the whole fusings of aluminium on pulvis surface, ZrO
2with the high temperature aluminum liquid of melting at ZrO
2particle surface reacts and generates Al
3zr and Al
2o
3reinforcement, by compounding flux refining, degasification, skim and inoculation after pour in ready mould, can obtain required (Al
3zr+Al
2o
3)/Al matrix material, is illustrated in figure 4 (the Al of preparation
3zr+Al
2o
3)/Al microstructure of composite photo.
Embodiment 2
With ZrO
2and B
2o
3for reaction pulvis original position preparation (ZrB
2+ Al
2o
3)/2024Al matrix material.
By analytical pure ZrO
2powder and B
2o
3the mixture of powder (mol ratio 1:1) (30vol.%) and middle particle diameter be that spherical 2024Al powder (70vol.%) ball milling of 25 μ m mixes, colds pressing, sintering acquisition compound powder sintered blank, sintering temperature is 680 ℃, sintering time is 2h, and concrete steps are identical with embodiment 1; The 2024Al ingot casting that is 500g by quality is put into crucible oven and is melted and be incubated to 870 ℃, then compound powder sintered blank is put into molten aluminium and apply ultrasonication carry out compound, power 500W, ultrasonic 30min, the final (ZrB that obtains
2+ Al
2o
3)/2024Al matrix material, concrete steps are identical with embodiment 1.
Embodiment 3
With TiO
2and B
4c is reaction pulvis original position preparation (TiB
2+ TiC+Al
2o
3)/6061Al matrix material.
By analytical pure TiO
2powder and B
4the mixture of C powder (mol ratio 3:1) (30vol.%) and middle particle diameter is that spherical 6061Al powder (70vol.%) ball milling of 25 μ m mixes, colds pressing, sintering and with the compound preparation (TiB of 6061Al melt
2+ TiC+Al
2o
3)/6061Al matrix material, concrete steps are identical with embodiment 2; Sintering temperature is 720 ℃, and sintering time is 1.5h, as the Heating temperature of 6061 alloys of matrix, is 900 ℃, power 1000W, ultrasonic 20min.
Claims (7)
1. an aluminum based composite material enhanced by granules in situ preparation method, is characterized in that comprising the steps:
(1) preparation of compound powder blank: the pottery reaction pulvis of reactionless by product and aluminium powder are adopted to ball milling
Method is evenly mixed and is cold-pressed into base, is then placed in atmosphere or vacuum oven sintering, and the aluminium powder in pressed compact is melted
And Host range pulvis obtains sintered blank;
(2) ultrasonic dispersion is compound: the fine aluminium as matrix or its alloy are heated to pulvis temperature of reaction insulation,
Then sintered blank is dropped in molten aluminium, melt is applied to ul-trasonic irradiation simultaneously, by hyperacoustic cavitation,
Acoustic streaming effect promotes the carrying out of the stirring of melt, the dispersion of pulvis and reaction;
(3) molding component: the Composite Melt obtaining is carried out after refining, slagging-off, degasification and inoculation,
Adopt the method for liquid condition shaping to obtain composite element.
2. a kind of aluminum based composite material enhanced by granules in situ preparation method as claimed in claim 1, is characterized in that described reaction pulvis, is ZrO
2ceramic powder, TiO
2the ZrO of ceramic powder, mol ratio 1:1
2and B
2o
3mixture, the ZrO of mol ratio 1:2
2with the mixture of B, the TiO of mol ratio 1:1
2and B
2o
3mixture, the TiO of mol ratio 1:2
2with the mixture of B or the TiO of mol ratio 3:1
2and B
4the mixture of C; The content of its reaction pulvis is for the pottery reaction pulvis of ball milling and 20 ~ 50vol.% of aluminium powder cumulative volume.
3. a kind of aluminum based composite material enhanced by granules in situ preparation method as claimed in claim 1, is characterized in that: described in be cold-pressed into base the pressure of colding pressing be 300MPa, the base density of colding pressing is 70% ~ 85%.
4. a kind of aluminum based composite material enhanced by granules in situ preparation method as claimed in claim 1, is characterized in that: described aluminium powder is identical with matrix composition, a kind of in fine aluminium or its alloy, and the particle diameter of aluminium powder is 2 ~ 50 μ m.
5. a kind of aluminum based composite material enhanced by granules in situ preparation method as claimed in claim 1, it is characterized in that: described ball milling, object is the even mixing of realization response pulvis and reinforcement, adopt 1-S lab stirring ball mill, rotational speed of ball-mill is 426r/min, ratio of grinding media to material is 20:1, Ball-milling Time 1h.
6. a kind of aluminum based composite material enhanced by granules in situ preparation method as claimed in claim 1, is characterized in that: described sintering temperature is above 50 ~ 150 ℃ of matrix alloy fusing point, and sintering time is 0.5 ~ 2h.
7. a kind of aluminum based composite material enhanced by granules in situ preparation method as claimed in claim 1, is characterized in that: described is ultrasonic, and its parameter is velocity of wave 1500m/s, frequency 20kHz, power 500 ~ 1500W, time 10 ~ 30min.
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Cited By (6)
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| CN105002385A (en) * | 2015-08-04 | 2015-10-28 | 北京科技大学 | Method for increasing sintering density of ceramic particle enhanced Al-based composite material |
| CN104999074A (en) * | 2015-08-04 | 2015-10-28 | 北京科技大学 | Method for improving sintered density of aluminum alloy powder metallurgy part |
| CN109550963A (en) * | 2018-12-13 | 2019-04-02 | 华南理工大学 | A kind of sub-micron hydride particle enhancing aluminium base raw powder's production technology for 3D printing |
| CN110331311A (en) * | 2019-04-22 | 2019-10-15 | 江苏大学 | A kind of continuous preparation method of in-situ ceramic particle enhanced aluminum-based composite material |
| CN111020300A (en) * | 2019-12-05 | 2020-04-17 | 江苏大学 | Preparation method of thermal cracking resistant binary nanoparticle reinforced aluminum matrix composite |
| CN114990415A (en) * | 2022-06-15 | 2022-09-02 | 中国重汽集团济南动力有限公司 | Nano biphase reinforced aluminum-based composite material and 3D printing forming method thereof |
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| CN105002385A (en) * | 2015-08-04 | 2015-10-28 | 北京科技大学 | Method for increasing sintering density of ceramic particle enhanced Al-based composite material |
| CN104999074A (en) * | 2015-08-04 | 2015-10-28 | 北京科技大学 | Method for improving sintered density of aluminum alloy powder metallurgy part |
| CN109550963A (en) * | 2018-12-13 | 2019-04-02 | 华南理工大学 | A kind of sub-micron hydride particle enhancing aluminium base raw powder's production technology for 3D printing |
| CN110331311A (en) * | 2019-04-22 | 2019-10-15 | 江苏大学 | A kind of continuous preparation method of in-situ ceramic particle enhanced aluminum-based composite material |
| CN111020300A (en) * | 2019-12-05 | 2020-04-17 | 江苏大学 | Preparation method of thermal cracking resistant binary nanoparticle reinforced aluminum matrix composite |
| CN114990415A (en) * | 2022-06-15 | 2022-09-02 | 中国重汽集团济南动力有限公司 | Nano biphase reinforced aluminum-based composite material and 3D printing forming method thereof |
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Application publication date: 20140917 Assignee: Nantong Jiangzhong Photoelectricity Co., Ltd. Assignor: Jiangsu University Contract record no.: 2019320000028 Denomination of invention: Preparation method of in-situ particle reinforced aluminum-based composite material Granted publication date: 20160525 License type: Exclusive License Record date: 20190311 |