CN103173645A - Preparation method of dispersedly strengthened aluminum-based composite material - Google Patents

Preparation method of dispersedly strengthened aluminum-based composite material Download PDF

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CN103173645A
CN103173645A CN2013100966614A CN201310096661A CN103173645A CN 103173645 A CN103173645 A CN 103173645A CN 2013100966614 A CN2013100966614 A CN 2013100966614A CN 201310096661 A CN201310096661 A CN 201310096661A CN 103173645 A CN103173645 A CN 103173645A
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cuo
melt
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matrix composite
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CN103173645B (en
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郭志猛
陈存广
罗骥
陈骏
王雯雯
郝俊杰
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Tian Ti Long (tianjin) Metal Material Co Ltd
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University of Science and Technology Beijing USTB
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Abstract

The invention discloses a preparation method of a dispersedly strengthened aluminum-based composite material, and belongs to the field of the preparation of the aluminum-based composite material. A strengthened particle is derived from CuO/Al2O3 nanometer composite powder prepared by means of sol-gel method. The method comprises the following steps of: melting industrial pure aluminum or an aluminum alloy, and carrying out degassing and slag removal treatment on the molten product to obtain a clean pure aluminum melt or a clean aluminum alloy melt; adding the CuO/Al2O3 nanometer composite powder into the pure aluminum melt or the aluminum alloy melt in batches under the stirring action at 750-850 DEG C to obtain a composite melt, and then carrying out high-energy ultrasonic treatment on the composite melt, wherein the amount of the CuO/Al2O3 nanometer composite powder is 0.2wt.%-2.0wt.% of that of the composite melt; and reducing the temperature of the composite melt to 680-720 DEG C, casting the resulting composite melt to a preheated metal mold at 250-300 DEG C, cooling the mold and carrying out mold release to obtain the dispersedly strengthened aluminum-based composite material. The preparation method disclosed by the invention is simple and stable in process, convenient for operation and low in production cost, interface bonding of enhancing particles with an alloy matrix is good, the enhancing particles are uniformly and dispersedly distributed in the matrix, and the performance of the composite material is excellent.

Description

A kind of preparation method of dispersion-strengthened aluminum matrix composite
Technical field
The invention belongs to the aluminum matrix composite preparing technical field, a kind of preparation method of nano particle dispersion-strengthened aluminum matrix composite particularly is provided.
Technical background
Excellent physicals and the mechanical properties such as that aluminum matrix composite has is lightweight, specific tenacity is high, specific modulus is high, thermal expansivity is low, high temperature resistant, wear-resistant, dimensional stabilizing are widely used in the fields such as aerospace, military and national defense and communications and transportation, Electronic Packaging.Wherein, the dispersion-strengthened aluminum matrix composite has the characteristics such as cost is low, preparation technology simple, performance is more outstanding, becomes gradually the study hotspot in domestic and international aluminum matrix composite field.Dispersion-strengthened aluminum matrix composite technology of preparing commonly used has powder metallurgic method and two kinds of techniques of casting.The complex process equipment of powder metallurgic method, high expensive are difficult for preparation large volume and complex-shaped part, and have in process of production the danger such as dust-firing and blast.And casting technique is simple, and is easy to operate, can prepare the matrix material of large volume, and equipment investment is few, and production cost is low, and productivity is high, the suitability for industrialized scale production.
Traditional aluminum matrix composite is that enhanced granule is applied in aluminum substrate, to exist between enhanced granule and matrix wettability poor owing to adding particle in aluminum substrate, surface reaction is difficult to control, and the defectives such as enhanced granule skewness have affected the performance of aluminum matrix composite.How to improve the wettability between enhanced granule and matrix, improve the interface performance of material, become when previous problem demanding prompt solution.
The high-energy ultrasonic method be a kind of with nanoparticulate dispersed the effective ways in the aluminium alloy melt.The high-energy ultrasonic ratio juris is to utilize sound cavitation effect that ultrasonic wave produces in aluminium alloy melt and the stirring in the caused mechanics effect of acoustic streaming effect, dispersion, degasification etc. to be used for promoting nano particle to sneak into aluminium alloy melt; improve the wettability between nano particle and aluminium alloy melt, force nano particle Uniform Dispersion in aluminium alloy melt.The high-energy ultrasonic method is the preparation method of a kind of simple process, dispersion-strengthened aluminum matrix composite with low cost.But, according to conventional cast technique, single enhanced granule being applied in aluminium alloy melt, most of enhanced granule can float over bath surface or adhere to the smelting pot inwall in the high-energy ultrasonic dispersion process, is difficult for Uniform Dispersion and enters in whole aluminium alloy melt.Therefore, disperse inhomogeneously in the final aluminum matrix composite that obtains on the enhanced granule macroscopic view, consistency of performance is poor.
Summary of the invention
The object of the invention is to overcome disperse on the enhanced granule macroscopic view in the aluminum matrix composite that prior art exists inhomogeneous, the problem that consistency of performance is poor, a kind of preparation method of dispersion-strengthened aluminum matrix composite is provided, the dispersion-strengthened aluminum matrix composite exists fragility phase and the inhomogeneous defective of distribution of material, nano level Al to make it solve in the past 2O 3Particle evenly distributes in matrix, has played dispersion-strengthened action, and the strength and modulus of matrix is improved significantly.
At first a kind of preparation method of dispersion-strengthened aluminum matrix composite adopts sol-gel method to prepare CuO/Al 2O 3Nano composite powder makes nanometer Al 2O 3Mix with the CuO uniform particles, to guarantee nanometer Al 2O 3The follow-up abundant dispersion of particle enters aluminium alloy melt inside, then adopts the standby dispersion-strengthened aluminum matrix composite of high-energy ultrasonic legal system.Concrete grammar comprises following content:
1, sol-gel method prepares CuO/Al 2O 3Nano composite powder
(1) with soluble copper salt and exsiccated ammonium alum (NH 4Al (SO 4) 2) be raw material, be mixed with the aqueous solution of 0.1～25 mol/L as reaction mother liquor, prepare certain density bicarbonate of ammonia (NH 4HCO 3) solution is as precipitation agent, according to CuO/Al 2O 3Middle Al 2O 3Content is determined mantoquita and exsiccated ammonium alum (NH 4Al (SO 4) 2) amount, according to NH 4Al (SO 4) 2With NH 4HCO 3Mol ratio be 1:4 and Cu 2+With NH 4HCO 3Mol ratio be that 1:2 determines NH 4HCO 3Amount.
(2) precipitant solution is added in reaction mother liquor, add 0.5～1.0 mol/L NH simultaneously in reaction system 3H 2It is neutral that O regulation system pH value remains, after continuing to stir 10～60 min, ultra-sonic dispersion 5～30 min obtain the water-sol, and stirring velocity is 100～500 r/min, and ultrasonic power is 100～1000 W.
(3) with after above-mentioned gained water-sol ageing 10～24 h, remove supernatant liquid, get gel after centrifuge dehydration.Pulverize after under 80 ℃, gel being dried, calcine 60～120 min and namely get CuO/Al in 500～800 ℃ of air 2O 3Nano composite powder.
2, the standby dispersion-strengthened aluminum matrix composite of high-energy ultrasonic legal system
(1) the technical pure aluminum or aluminum alloy is placed in crucible electrical resistance furnace, is warming up to higher than 50～80 ℃ of technical pure aluminum or aluminum alloy fusing points and makes its fusing, after processing through the degasification slagging-off, obtain clean fine aluminium or aluminium alloy melt.
(2) continue to be warming up to 750～850 ℃, with the CuO/Al of aluminium foil parcel 2O 3Nano composite powder pushes melt inside with the graphite sleeve, turn on agitator simultaneously, and stirring velocity is 500～1000 r/min, churning time is 10～30 min, obtains compounding flux.
(4) high-energy ultrasonic is processed compounding flux, and frequency is 17～20 KHz, and peak power output is 1～2 KW, and the treatment time is 5～30 min.
(5) above-mentioned compounding flux is cooled to 680～720 ℃, is poured in the metal type dies of 250～300 ℃ of preheatings, the cooling rear demoulding namely gets the dispersion-strengthened aluminum matrix composite.
Step a(1) CuO/Al described in 2O 3Al in nano composite powder 2O 3Content is 10wt.%～90 wt.%.
Step a(1) soluble copper salt described in comprises any one or a few in copper sulfate, cupric chloride, cupric nitrate.
Step b(1) aluminium alloy described in can be any one or a few during Al-Si, Al-Cu, Al-Mg, Al-Zn are.
Step b(2) CuO/Al described in 2O 3The add-on of nano composite powder is the 0.2wt.%～2.0 wt.% of dispersion-strengthened aluminum matrix composite.
Step b(2) CuO/Al described in 2O 3Nano composite powder add mode for add in batches, be divided into 2～5 equal portions.
Compared with prior art, superiority of the present invention is:
(1) adopt sol-gel method to prepare CuO/Al 2O 3Nano composite powder makes nanometer Al 2O 3Mix with the CuO uniform particles, guarantee on the one hand nanometer Al 2O 3The follow-up abundant dispersion of particle enters aluminium alloy melt inside, on the other hand when nanometer CuO and molten aluminium generation thermite reaction, due to Al 2O 3The existence of particle is played certain " solid diluting effect " to nanometer CuO powder, prevents that reaction process from blasting, and the Cu that thermite reaction generates plays solution strengthening effect, has improved simultaneously Al 2O 3The interface wet ability of particle and aluminum substrate, thus the interface performance of matrix material improved.
(2) utilize the graphite sleeve with CuO/Al 2O 3Nano composite powder pushes melt inside, has solved the problem that enhanced granule that traditional enhanced granule mode that adds produces floats over bath surface or adheres to the smelting pot inwall.
(3) under the high-energy ultrasonic effect, the rolling disturbance that utilizes simultaneously violent surface reaction to form realizes the nanometer Al that surface reaction generates 2O 3Particle and CuO/Al 2O 3The nanometer Al that nano composite powder is directly introduced 2O 3The disperse of particle in whole aluminium alloy melt distributes, and strengthening effect further strengthens.
(4) adopt the aluminum matrix composite of the inventive method preparation, have the performance of high abrasion, high tenacity, have a extensive future.
Embodiment
Embodiment 1
(1) sol-gel method prepares CuO/Al 2O 3Nano composite powder: preparation 0.1 mol/L CuSO 4, 1.4 mol/L NH 4Al (SO 4) 2) the aqueous solution as reaction mother liquor, the preparation 5.8 mol/L NH 4HCO 3Solution adds 500 ml precipitant solution in 500 ml reaction mother liquors as precipitation agent, adds 0.5 mol/L NH simultaneously in reaction system 3H 2It is neutral that O regulation system pH value remains, with ultra-sonic dispersion 5 min after the lasting stirring of 100 r/min stirring velocitys 10 min, ultrasonic power is 100 W.After above-mentioned gained water-sol ageing 10 h, remove supernatant liquid, get gel after centrifuge dehydration.Pulverize after under 80 ℃, gel being dried, calcining 60 min namely get CuO/Al in 500 ℃ of air 2O 3Nano composite powder, wherein Al 2O 3Content is 90wt.%.
(2) the standby dispersion-strengthened aluminum matrix composite of high-energy ultrasonic legal system: 500 g commercial-purity aluminiums are placed in crucible electrical resistance furnace, are warming up to 710 ℃ and make its fusing, after processing through the degasification slagging-off, obtain clean melt.Continue to be warming up to 750 ℃, with 10 g CuO/Al 2O 3Nano composite powder is divided equally 5 parts, pushes molten aluminium inside with the graphite sleeve after aluminium foil parcel, stirs 10 min with 1000 r/min stirring velocitys, acquisition clad aluminum melt.Afterwards the clad aluminum melt is applied supersound process 30 min of frequency 20 KHz, peak power output 1 KW.Above-mentioned melt is cooled to 680 ℃, is poured in the metal type dies of 250 ℃ of preheatings, the cooling rear demoulding namely gets the dispersion-strengthened aluminum matrix composite.
Embodiment 2
(1) sol-gel method prepares CuO/Al 2O 3Nano composite powder: preparation 5.8 mol/L Cu (NO 3) 2, 10 mol/L NH 4Al (SO 4) 2) the aqueous solution as reaction mother liquor, the preparation 51.6 mol/L NH 4HCO 3Solution adds 500 ml precipitant solution in 500 ml reaction mother liquors as precipitation agent, adds 1.0 mol/L NH simultaneously in reaction system 3H 2It is neutral that O regulation system pH value remains, with ultra-sonic dispersion 30 min after the lasting stirring of 500 r/min stirring velocitys 60 min, ultrasonic power is 1000 W.After above-mentioned gained water-sol ageing 24 h, remove supernatant liquid, get gel after centrifuge dehydration.Pulverize after under 80 ℃, gel being dried, calcining 120 min namely get CuO/Al in 900 ℃ of air 2O 3Nano composite powder, wherein Al 2O 3Content is 10wt.%.
(2) the standby dispersion-strengthened aluminum matrix composite of high-energy ultrasonic legal system: 800 g 2024 aluminium alloys are placed in crucible electrical resistance furnace, are warming up to 750 ℃ and make its fusing, after processing through the degasification slagging-off, obtain clean melt.Continue to be warming up to 850 ℃, with 1.6 g CuO/Al 2O 3Nano composite powder is divided equally 2 parts, pushes molten aluminium inside with the graphite sleeve after aluminium foil parcel, stirs 30 min with 500 r/min stirring velocitys, acquisition clad aluminum melt.Afterwards the clad aluminum melt is applied supersound process 5 min of frequency 17 KHz, peak power output 2 KW.Above-mentioned melt is cooled to 700 ℃, is poured in the metal type dies of 300 ℃ of preheatings, the cooling rear demoulding namely gets the dispersion-strengthened aluminum matrix composite.
Embodiment 3
(1) sol-gel method prepares CuO/Al 2O 3Nano composite powder: preparation 3.2 mol/L CuCl 2, 5 mol/L NH 4Al (SO 4) 2) the aqueous solution as reaction mother liquor, the preparation 26.4 mol/L NH 4HCO 3Solution adds 500 ml precipitant solution in 500 ml reaction mother liquors as precipitation agent, adds 0.8 mol/L NH simultaneously in reaction system 3H 2It is neutral that O regulation system pH value remains, with ultra-sonic dispersion 20 min after the lasting stirring of 300 r/min stirring velocitys 30 min, ultrasonic power is 600 W.After above-mentioned gained water-sol ageing 18 h, remove supernatant liquid, get gel after centrifuge dehydration.Pulverize after under 80 ℃, gel being dried, calcining 90 min namely get CuO/Al in 750 ℃ of air 2O 3Nano composite powder, wherein Al 2O 3Content is 50wt.%.
(2) the standby dispersion-strengthened aluminum matrix composite of high-energy ultrasonic legal system: 400 g 6063 aluminium alloys are placed in crucible electrical resistance furnace, are warming up to 730 ℃ and make its fusing, after processing through the degasification slagging-off, obtain clean melt.Continue to be warming up to 800 ℃, with 4 g CuO/Al 2O 3Nano composite powder is divided equally 4 parts, pushes molten aluminium inside with the graphite sleeve after aluminium foil parcel, stirs 20 min with 800 r/min stirring velocitys, acquisition clad aluminum melt.Afterwards the clad aluminum melt is applied supersound process 15 min of frequency 19 KHz, peak power output 1.5 KW.Above-mentioned melt is cooled to 720 ℃, is poured in the metal type dies of 300 ℃ of preheatings, the cooling rear demoulding namely gets the dispersion-strengthened aluminum matrix composite.

Claims (6)

1. the preparation method of a dispersion-strengthened aluminum matrix composite, is characterized in that, preparation process comprises:
A, sol-gel method prepare CuO/Al 2O 3Nano composite powder
(1) with soluble copper salt and NH 4Al (SO 4) 2Be raw material, be mixed with the aqueous solution of 0.1～25 mol/L as reaction mother liquor, prepare certain density NH 4HCO 3Solution is as precipitation agent, according to CuO/Al 2O 3Middle Al 2O 3Content is determined mantoquita and NH 4Al (SO 4) 2Amount, according to NH 4Al (SO 4) 2With NH 4HCO 3Mol ratio be 1:4 and Cu 2+With NH 4HCO 3Mol ratio be that 1:2 determines NH 4HCO 3Amount;
(2) precipitant solution is added in reaction mother liquor, add 0.5～1.0 mol/L NH simultaneously in reaction system 3H 2It is neutral that O regulation system pH value remains, after continuing to stir 10～60 min, ultra-sonic dispersion 5～30 min obtain the water-sol, and stirring velocity is 100～500 r/min, and ultrasonic power is 100～1000 W;
(3) with after step (2) gained water-sol ageing 10～24 h, remove supernatant liquid, get gel after centrifuge dehydration, pulverize after under 80 ℃, gel being dried, calcine 60～120 min and namely get CuO/Al in 500～800 ℃ of air 2O 3Nano composite powder;
B, the standby dispersion-strengthened aluminum matrix composite of high-energy ultrasonic legal system
(1) the technical pure aluminum or aluminum alloy is placed in crucible electrical resistance furnace, is warming up to higher than 50～80 ℃ of technical pure aluminum or aluminum alloy fusing points and makes its fusing, after processing through the degasification slagging-off, obtain clean fine aluminium or aluminium alloy melt;
(2) continue to be warming up to 750～850 ℃, with the CuO/Al of aluminium foil parcel 2O 3Nano composite powder pushes melt inside with the graphite sleeve, turn on agitator simultaneously, and stirring velocity is 500～1000 r/min, churning time is 10～30 min, obtains compounding flux;
(4) high-energy ultrasonic is processed compounding flux, and frequency is 17～20 KHz, and peak power output is 1～2 KW, and the treatment time is 5～30 min;
(5) step (5) gained compounding flux is cooled to 680～720 ℃, is poured in the metal type dies of 250～300 ℃ of preheatings, the cooling rear demoulding namely gets the dispersion-strengthened aluminum matrix composite.
2. the preparation method of dispersion-strengthened aluminum matrix composite according to claim 1, is characterized in that step a(1) described in CuO/Al 2O 3Al in nano composite powder 2O 3Content is 10wt.%～90 wt.%.
3. the preparation method of dispersion-strengthened aluminum matrix composite according to claim 1, is characterized in that step a(1) described in soluble copper salt comprise any one or a few in copper sulfate, cupric chloride, cupric nitrate.
4. the preparation method of dispersion-strengthened aluminum matrix composite according to claim 1, is characterized in that step b(1) described in aluminium alloy can be any one or a few in Al-Si, Al-Cu, Al-Mg, Al-Zn system.
5. the preparation method of dispersion-strengthened aluminum matrix composite according to claim 1, is characterized in that step b(2) described in CuO/Al 2O 3The add-on of nano composite powder is the 0.2wt.%～2.0 wt.% of dispersion-strengthened aluminum matrix composite.
6. the preparation method of dispersion-strengthened aluminum matrix composite according to claim 1, is characterized in that step b(2) described in CuO/Al 2O 3Nano composite powder add mode for add in batches, be divided into 2～5 equal portions.
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104131186A (en) * 2014-08-16 2014-11-05 孟红琳 Method for preparing aluminum-based composite material subjected to enhanced particle-copper alloy interface compatibility treatment
CN105506328A (en) * 2015-12-17 2016-04-20 梅庆波 Preparation method for magnesium-based aluminum iron composite material
CN105537310A (en) * 2015-12-17 2016-05-04 梅庆波 Preparation method of aluminium alloy profile
CN105834609A (en) * 2016-05-04 2016-08-10 桂林市庆通有色金属工艺材料开发有限公司 Continuous brazing composite aluminum-based brazing wire applying nanometer aluminum trioxide and preparation method of continuous brazing composite aluminum-based brazing wire applying nanometer aluminum trioxide
CN108251685A (en) * 2018-01-22 2018-07-06 北京科技大学 A kind of tungsten dispersed and strengthened copper-based composite material and preparation method thereof
CN109396422A (en) * 2018-12-27 2019-03-01 吉林大学 A kind of method evenly dispersed in the pre-dispersed complementary melt of nano particle in parcel
CN110791613A (en) * 2019-09-30 2020-02-14 鞍钢股份有限公司 Method for adding nano particles into steel, refining structure of nano particles and strengthening and toughening steel
CN111057979A (en) * 2019-12-17 2020-04-24 北京科技大学 Composite physical field regulation and control method for original phase dispersion of high-performance aluminum alloy for vehicle
CN115404388A (en) * 2022-09-08 2022-11-29 山东创新精密科技有限公司 Composite reinforced aluminum alloy material and preparation method thereof
CN115418520A (en) * 2022-06-28 2022-12-02 江苏大学 In-situ Al 2 O 3 Preparation method of particle reinforced aluminum matrix composite

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CN1900332A (en) * 2006-07-22 2007-01-24 淮阴工学院 Method for preparing copper base composite material by chemical precipitation method to obtain composite powder
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JPH01138133A (en) * 1987-11-24 1989-05-31 Neos Co Ltd Production of complex oxide containing copper oxide utilizing sol-gel transformation
CN1900332A (en) * 2006-07-22 2007-01-24 淮阴工学院 Method for preparing copper base composite material by chemical precipitation method to obtain composite powder
CN101015808A (en) * 2007-02-25 2007-08-15 汕头大学 Nm-class catalyst for transforming NO to N2 and its preparing process

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104131186A (en) * 2014-08-16 2014-11-05 孟红琳 Method for preparing aluminum-based composite material subjected to enhanced particle-copper alloy interface compatibility treatment
CN105506328A (en) * 2015-12-17 2016-04-20 梅庆波 Preparation method for magnesium-based aluminum iron composite material
CN105537310A (en) * 2015-12-17 2016-05-04 梅庆波 Preparation method of aluminium alloy profile
CN105834609A (en) * 2016-05-04 2016-08-10 桂林市庆通有色金属工艺材料开发有限公司 Continuous brazing composite aluminum-based brazing wire applying nanometer aluminum trioxide and preparation method of continuous brazing composite aluminum-based brazing wire applying nanometer aluminum trioxide
CN108251685A (en) * 2018-01-22 2018-07-06 北京科技大学 A kind of tungsten dispersed and strengthened copper-based composite material and preparation method thereof
CN108251685B (en) * 2018-01-22 2020-04-07 北京科技大学 Tungsten dispersion strengthening copper-based composite material and preparation method thereof
CN109396422A (en) * 2018-12-27 2019-03-01 吉林大学 A kind of method evenly dispersed in the pre-dispersed complementary melt of nano particle in parcel
CN110791613A (en) * 2019-09-30 2020-02-14 鞍钢股份有限公司 Method for adding nano particles into steel, refining structure of nano particles and strengthening and toughening steel
CN111057979A (en) * 2019-12-17 2020-04-24 北京科技大学 Composite physical field regulation and control method for original phase dispersion of high-performance aluminum alloy for vehicle
CN111057979B (en) * 2019-12-17 2021-06-29 北京科技大学 Composite physical field regulation and control method for original phase dispersion of high-performance aluminum alloy for vehicle
CN115418520A (en) * 2022-06-28 2022-12-02 江苏大学 In-situ Al 2 O 3 Preparation method of particle reinforced aluminum matrix composite
CN115404388A (en) * 2022-09-08 2022-11-29 山东创新精密科技有限公司 Composite reinforced aluminum alloy material and preparation method thereof

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