CN108359823B - A kind of preparation method of in-situ preparation MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy - Google Patents

A kind of preparation method of in-situ preparation MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy Download PDF

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CN108359823B
CN108359823B CN201810314755.7A CN201810314755A CN108359823B CN 108359823 B CN108359823 B CN 108359823B CN 201810314755 A CN201810314755 A CN 201810314755A CN 108359823 B CN108359823 B CN 108359823B
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powder
alloy
ball
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CN108359823A (en
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周登山
张德良
耿宏伟
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Northeastern University China
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Northeastern University China
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0408Light metal alloys
    • C22C1/0416Aluminium-based alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/06Alloys based on aluminium with magnesium as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/002Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/047Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with magnesium as the next major constituent

Abstract

The invention belongs to field of powder metallurgy, and in particular to a kind of preparation method of in-situ preparation MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy.Technical scheme is as follows: including the following steps: to weigh Al powder and Mg powder, wherein the atomic ratio of alloy shared by solute Mg atom is 0-8at.%;Ball milling is sufficiently mixed under the low speed of service powder 6 hours first with planetary ball mill, and revolving speed is 180-220 revs/min;Then again at high running speeds to mixed-powder ball milling 36 hours, revolving speed is 480-520 revs/min, Non-intermittent during high-energy ball milling;Passivation Treatment is pressed into powder base;500 DEG C are heated to, then keeps the temperature 2 minutes at 500 DEG C, after keeping the temperature, the powder base of heating is moved into immediately in the extrusion die of preheating and powder base is hot extruded into the hot extrusion pressure bar for diameter 6mm;Heat treatment.Alloy prepared by the present invention has the advantages that low-density, high intensity, high elastic modulus, ultra-fine microstructure and cleaning granular boundary.

Description

A kind of preparation method of in-situ preparation MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy
Technical field
The invention belongs to field of powder metallurgy, and in particular to a kind of in-situ preparation MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy Preparation method.
Background technique
Al-Mg alloy is answered extensively because of its low-density, excellent corrosion resistance, welding performance and good comprehensive mechanical property For aerospace, marine ship and auto industry.However, since the solid solution that the intensity of the alloy mostlys come from Mg element is strong Change, so, the intensity of alloy and the concentration for the solute Mg atom being dissolved in Al matrix are closely related.But traditional ingot casting smelting In 5~6wt.% (mass percent) left and right, which is only capable of mentioning Mg constituent content in the Al-Mg light-alloy of golden method preparation Increase for limited intensity;In addition, the addition of Mg element also reduces the elasticity modulus of Al.It therefore, is expansion Al-Mg light-alloy Application range and meet some extreme Service Environments, its intensity and modulus need to be improved.
Refinement crystal grain and addition/introducing the second phase fine particle are strengthening material and the classical way for improving its modulus.Base In such understanding and understanding, the crystallite dimension of Al-Mg light-alloy is refine to Ultra-fine Grained (100 nanometers of < average grain sizes 1 micron of <) range and thereto introduce Nano grade the second ceramic phase particle will certainly significantly improve material intensity and Elasticity modulus.The method of known refinement cast metals material microstructure specifically include that Static Recrystallization (room temperature or cold deformation+ Heat treatment), dynamic recrystallization (temperature or thermal deformation) and severe plastic deformation (waiting channel pressings and high pressure torsion) etc..Using above-mentioned Method prepares super fine crystal material, and material is generally required to have high plastic deformation ability.However, for ingot casting Al-Mg alloy, The plastic deformation ability of alloy is dissolved Mg atom content by it and is limited, after solute Mg atom content is more than 5.5wt.%, modeling Property deformability sharply declines, and leads to not carry out necessary deformation processing to it to obtain hyperfine structure.If containing again to high magnesium Second Phase Particle is added in amount ingot casting Al-Mg alloy, the deformability of alloy can become even worse, and it is even more impossible to carry out plasticity change to it Shape processing.Therefore, high-strength high-elasticity modulus Second Phase Particle dispersion-strengtherning Ultra-fine Grained Al-Mg alloy is difficult with conventional method To prepare.
The exploitation that traditional Second Phase Particle strengthens Al-Mg composite material is related to Semi-solid Stirring casting, stirring casting, ultrasound Assisted casting and pressure-free impregnation etc..Common Second Phase Particle includes: SiC, Al2O3And B4C particle etc..It has following insufficient:
1) microstructure of Al-Mg alloy substrate is coarse.
2) Second Phase Particle size is larger and small volume.
3) Second Phase Particle is easy to reunite and forms particle clusters.
4) alloy substrate and granular boundary, which easily react, generates brittlement phase.
5) strength of materials and elasticity modulus are still relatively low.
Mechanic Alloying Technology can realize the severe plastic deformation and repeatedly of metal ductility powder using superpower mechanical energy Powder fracture, cold welding, after certain time mechanical alloying, the microstructure of metal powder can be refined to nano-scale.Machine Tool alloying can not only realize the nanosizing of metal powder, moreover it is possible to efficiently, equably disperse the second phase nano particle to nano junction In structure metal powder.In conjunction with traditional powder metallurgy consolidation means (such as sintering, hot pressing, warm and hot forging and hot extrusion), machinery is closed Aurification metal powder can be used to prepare hyperfine structure metal sample and components.
Summary of the invention
The present invention provides a kind of preparation method of in-situ preparation MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy, closes in conjunction with machinery Aurification technology and reaction in-situ principle, are prepared for MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy in situ, the alloy have low-density, The advantages of high intensity, high elastic modulus, ultra-fine microstructure and cleaning granular boundary.
Technical scheme is as follows:
A kind of preparation method of in-situ preparation MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy, includes the following steps:
A. Al powder and Mg powder are weighed with precision balance, wherein the atomic ratio of alloy shared by solute Mg atom is 0- 8at.%;Select 1wt.% stearic acid as process control agent, to prevent and avoid the excessive cold welding of powder;
B. load weighted Al powder and Mg powder are put into the ball grinder equipped with stainless steel abrading-ball, the stainless steel abrading-ball is 5 The steel ball of a diameter 20mm and 10 diameter 16mm;Wherein, total matter of the gross mass of Al powder and Mg powder and the stainless steel abrading-ball The ratio of amount is 5:1;
C. in the glove box full of argon gas, operation is sealed to the ball grinder equipped with stainless steel abrading-ball and powder;
D. it is sufficiently mixed under the low speed of service with planetary ball mill powder 6 hours first, revolving speed is 180-220 revs/min Clock;Then again at high running speeds to mixed-powder ball milling 36 hours, revolving speed is 480-520 revs/min, nothing during high-energy ball milling Intermittently;
E. after high-energy ball milling, processing is passivated to the powder after ball milling in standard glove box, followed by liquid Powder after passivation is pressed into powder base under atmospheric environment by press;Powder base is the circle of diameter 28-30mm and high 25-35mm Column;
F. in the glove box full of argon gas that powder base is fast using the hydraulic press for being furnished with induction heating system and glove box Fast induction heating then keeps the temperature 2 minutes at 500 DEG C to 500 DEG C, after keeping the temperature, immediately moves into the powder base of heating The hot extrusion pressure bar for diameter 6mm is hot extruded into the extrusion die of preheating and by powder base;
G. hot extrusion pressure bar is placed in the 350-550 DEG C of heat treatment for carrying out 1-10 hours;The heat treatment parameter of use are as follows: heating 10 DEG C/min of rate, after being raised to the heat treatment temperature of setting, at such a temperature keep the temperature 5 hours, to soaking time after, stand Quenched into the water.
The present invention is the high activity using oxygen-containing metastable state Al-Mg alloy powder and magnesium elements, under the conditions of hot activation, Mg MgO nano particle is generated with O reaction in-situ.It is engaged in material science research and design of material developer is easy to think in the present invention It slightly expands, can obtain and material system of the material of the present invention without essential distinction on the basis of thinking.So protection of the invention Point will be covered: 1, utilizing the alloy powder of Al containing magnesium and internal oxidition/external oxidation method preparation MgO dispersion-strengtherning Al alloy material and Al base Composite material.2, using quickly solidifying oxygen-containing polynary Al alloy powder (containing magnesium) preparation MgO dispersion-strengtherning Al alloy material and Al Based composites.3, using different oxygen sources (metal oxide, process control agent or oxygen molecule) and the alloy powder of Al containing magnesium or The element powders of identical element ingredient carry out mechanical alloying to prepare MgO dispersion-strengtherning Al alloy material and Al base composite wood Material.
The invention has the benefit that
1, oxygen source is rich and varied, for example process control agent, is adsorbed on the oxygen molecule of powder particle surface or can be restored by Mg Metal oxide etc..
2, the process conditions, parameter of in-situ preparation MgO are easily realized and equipment is simple, are suitble to the production requirement of scale.
3, alloy has the features such as low-density, high intensity, high elastic modulus and high microstructure stability.
4, it can be used to prepare the Ultra-fine Grained Al-Mg based composites containing high MgO volume fraction.
5, reference is provided to prepare high-performance superfine crystalline substance Al-Mg based composites.
Detailed description of the invention
Fig. 1 is the microhardness of Al-Mg alloy sample with the variation relation figure of Mg content and heat treatment temperature, when heat treatment Between be 5 hours;
Fig. 2 is that the scanning transmission electron microscope of the Ultra-fine Grained Al-2.5at.%Mg alloy of 500 DEG C of heat treatment 5 hours is shone Piece and corresponding Mg, O element map;Wherein: (a), (b) be scanning transmission electron microscope photo, (c) be Mg element map, It (d) is O element map.
Specific embodiment
A kind of preparation method of in-situ preparation MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy, includes the following steps:
A. Al powder and Mg powder are weighed with precision balance, wherein the atomic ratio of alloy shared by solute Mg atom is respectively 0at.%, 2.5at.%, 5at.%, 7.5at.%;Select 1wt.% stearic acid as process control agent, to prevent and avoid powder The excessive cold welding in end;
B. load weighted Al powder and Mg powder are respectively put into the ball grinder equipped with stainless steel abrading-ball, the stainless steel abrading-ball For the steel ball of 5 diameter 20mm and 10 diameter 16mm;Wherein, the gross mass of Al powder and Mg powder and the stainless steel abrading-ball is total The ratio of quality is 5:1;
C. in the glove box full of argon gas, operation is sealed to the ball grinder equipped with stainless steel abrading-ball and powder;
D. it is sufficiently mixed under the low speed of service with planetary ball mill powder 6 hours first, revolving speed is 200 revs/min;So Afterwards again at high running speeds to mixed-powder ball milling 36 hours, revolving speed is 500 revs/min, Non-intermittent during high-energy ball milling;
E. after high-energy ball milling, processing is passivated to the powder after ball milling in standard glove box, followed by liquid Powder after passivation is pressed into powder base under atmospheric environment by press;Powder base is the cylinder of diameter 30mm and high 25mm;
F. in the glove box full of argon gas that powder base is fast using the hydraulic press for being furnished with induction heating system and glove box Fast induction heating then keeps the temperature 2 minutes at 500 DEG C to 500 DEG C, after keeping the temperature, immediately moves into the powder base of heating The hot extrusion pressure bar for diameter 6mm is hot extruded into the extrusion die of preheating and by powder base;
G. hot extrusion sample is cut from the hot extrusion pressure bar of heterogeneity respectively, and part hot extrusion sample is placed in 350- The heat treatment of 550 DEG C of progress 5 hours;The heat treatment parameter of use are as follows: 10 DEG C/min of heating rate, be raised to the heat treatment of setting After temperature, at such a temperature keep the temperature 5 hours, to soaking time after, be immediately placed in water carry out quenching obtain qtenched sample:
H. using epoxy resin and curing agent the hot extrusion sample of every kind of ingredient and qtenched sample edge at diameter 30mm and The cylinder of a height of 15mm inlays sample;After cylinder edge sample hardening, mechanical grinding and polishing treatment are carried out to it;Mechanical grinding process In, it is successively polished first using #300, #600, #1200, #2000 and #5000SiC sand paper, then with 5 μm of diamond Suspension is for further processing, and finally uses the SiO of 50nm2Suspension makees last finishing polish processing, polished machine when finishing polish Velocity of rotation is 150 revs/min;
I. the microhardness of cylinder edge sample in h step is measured, each cylinder edge sample at least measures 10 data points, lower pressure For 25g, the load time is 15 seconds, and the hardness number of measurement is as shown in Figure 1 with the variation relation of annealing temperature and cylinder edge sample ingredient;
J. the Ultra-fine Grained Al-2.5at.%Mg alloy of 500 DEG C of heat treatment 5 hours is characterized with scanning transmission electron microscope Sample, shown in (a) in the electromicroscopic photograph such as Fig. 2 of acquisition, (b);(c) and (d) confirms the presence of nano-MgO particle in Fig. 2.
The preparation method of material of the present invention is related to mechanical alloying, powder compact hot extrusion and heat treatment, belongs to powder smelting Golden collar domain.So can realize equifinality using obtained oxygen-containing Al-Mg alloyed powder is quickly solidified.Further, since Mg is extremely living It sprinkles, can be reacted with the metal oxide in-situ preparation nano-MgO particle of reduction activation after it or with added metal oxide Generate complex oxide.These are all in-situ preparation nano particles containing magnesium, are substantially no different with the present invention.In addition, the present invention selects Relatively simple binary Al-Mg alloy has been selected as matrix, as scientific research personnel and engineers and technicians, it is easy to expect adding Extra elements form polynary Al alloy substrate into binary Al-Mg alloy.Above situation can be on the basis of inventive idea Simple expand is carried out to achieve that.

Claims (1)

1. a kind of preparation method of in-situ preparation MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy, which is characterized in that including walking as follows It is rapid:
A. Al powder and Mg powder are weighed with precision balance, wherein the atomic ratio of alloy shared by solute Mg atom is 2.5-8at.%; Select 1wt.% stearic acid as process control agent, to prevent and avoid the excessive cold welding of powder;
B. load weighted Al powder and Mg powder are put into the ball grinder equipped with stainless steel abrading-ball, the stainless steel abrading-ball is 5 straight The steel ball of 20 mm and 10 16 mm of diameter of diameter;Wherein, the gross mass of the gross mass of Al powder and Mg powder and the stainless steel abrading-ball Ratio be 5:1;
C. in the glove box full of argon gas, operation is sealed to the ball grinder equipped with stainless steel abrading-ball and powder;
D. it is sufficiently mixed under the low speed of service with planetary ball mill powder 6 hours first, revolving speed is 180-220 revs/min;So Afterwards again at high running speeds to mixed-powder ball milling 36 hours, revolving speed is 480-520 revs/min, Non-intermittent during high-energy ball milling;
E. after high-energy ball milling, processing is passivated to the powder after ball milling in standard glove box, followed by hydraulic press The powder after passivation is pressed into powder base under atmospheric environment;Powder base is the cylinder of diameter 28-30mm and high 25-35mm;
F. using the hydraulic press for being furnished with induction heating system and glove box, powder base is quickly felt in the glove box full of argon gas 500 °C should be heated to, then keeps the temperature 2 minutes under 500 °C, after keeping the temperature, the powder base of heating is moved into preheating immediately Extrusion die in and powder base is hot extruded into the hot extrusion pressure bar for diameter 6mm;
G. hot extrusion pressure bar is placed in the 350-550 °C of heat treatment for carrying out 1-10 hours;The heat treatment parameter of use are as follows: heating rate 10 °C/minute, after being raised to the heat treatment temperature of setting, at such a temperature keep the temperature 5 hours, to soaking time after, put immediately Enter in water and is quenched.
CN201810314755.7A 2018-04-10 2018-04-10 A kind of preparation method of in-situ preparation MgO dispersion-strengtherning Ultra-fine Grained Al-Mg alloy Expired - Fee Related CN108359823B (en)

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CN110541083A (en) * 2019-09-06 2019-12-06 天津大学 Preparation method for in-situ synthesis of nano MgO reinforced aluminum alloy base composite material

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