CN107557706A - A kind of processing method for improving magnesium alloy strength - Google Patents

A kind of processing method for improving magnesium alloy strength Download PDF

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CN107557706A
CN107557706A CN201710785182.1A CN201710785182A CN107557706A CN 107557706 A CN107557706 A CN 107557706A CN 201710785182 A CN201710785182 A CN 201710785182A CN 107557706 A CN107557706 A CN 107557706A
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magnesium alloy
treatment
processing method
liquid nitrogen
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CN107557706B (en
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余晖
肖海涛
范少达
李丽超
丁俭
夏兴川
宋开红
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Hebei University of Technology
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Abstract

The present invention is a kind of processing method for improving magnesium alloy strength.This method comprises the following steps:1)As-cast magnesium alloy material is put into standing 5min ~ 24h in liquid nitrogen, or as-cast magnesium alloy material is put into liquid nitrogen after solution treatment, plastic deformation processing successively, stands 5min ~ 24h;2)Magnesium alloy materials after subzero treatment are taken out, are placed in air, clear-cutting forestland to room temperature.The present invention utilizes cryogenic treatment process, and the hardness of the system magnesium alloy can be significantly increased in a short time.The present invention has excellent treatment effect to high content Al or Sn magnesium alloy, so as to preferably meet industrial needs.

Description

A kind of processing method for improving magnesium alloy strength
Technical field
The present invention relates to a kind of heat treatment method for lifting high Sn or high Al contents magnesium alloy mechanical property, more particularly to A kind of processing method that wrought magnesium alloy intensity is improved using subzero treatment.
Background technology
Magnesium alloy is as most light structural metallic materials, and specific strength is high, shock resistance is good, can meet Aero-Space, Automobile and the light-weighted requirement of electronic product, energy resource consumption and environmental pollution are reduced, therefore should as developed country and regional industry With one of fastest-rising material.But compared with other materials, the mechanical property of current most of magnesium alloy is still relatively low how Improve the focus that its mechanical property is always studied both at home and abroad.Therefore, exploitation, which has inexpensive and high performance magnesium alloy concurrently, has Wide market prospects.
It is well known that alloying is to improve the effective means of material mechanical performance.Research shows, is added in magnesium alloy Rare earth element (RE) can prepare the magnesium alloy of excellent performance, but the factors such as preparation technology is complicated and on the high side strongly limit Its large-scale application, so the high-performance magnesium-alloy (such as Mg-Sn alloy systems) without rare earth element is increasingly subject to study at home and abroad The concern and attention of person.Have been reported and show that Mg-Sn alloy systems further can improve it by suitable Technology for Heating Processing Mechanical property, this is attributed to the invigoration effect that Ageing Treatment separates out a large amount of phases of disperse second, though addition Na elements are substantially shorter Reach peak value of hardness time, but its easily Grain Boundary Segregation deteriorate material plasticity (T.T.Sasaki, F.R.Elsayed, T.Nakata,T.Ohkubo,S.Kamado,K.Hono,Strong and ductile heat-treatable Mg-Sn-Zn- Al wrought alloys,Acta Materialia,2015(99):176-186. Cheng Wei are beautiful, fault Zhong Ping, Xu Chunxiang, Zhang Jin Mountain, Lin Fei, Liang Wei, a kind of high intensity reverse extrusion Mg-Sn based alloys and preparation method thereof Authorization Notice No.: CN102703785B).Can the intensity that raising Mg-Sn based alloys be reached using the Technology for Heating Processing of improvement be the pass for being badly in need of solving Key technical barrier.Being different from conventional aging strengthening model (T5 or T6) needs to be kept for the long period carry to reach at a certain temperature The method of high alloy intensity, by solid solution and Ageing Treatment, subzero treatment, ultrasonic impact handles and final Ageing Treatment, The intensity of magnesium alloy can be improved to a certain extent, and (Wang Zhanhong, Zhang Xunyin, Zhu Xiaohong, one kind improve magnesium alloy materials intensity and tough Property processing method publication numbers 201310453776.4), but length this method experimental period, treatment process steps are cumbersome, use instrument Device costly, directly increases production cost.As can be seen here, a kind of more simple, convenient, environmental protection, the raising of energy-conservation are developed The economical preparation method of Mg-Sn-Al-Zn magnesium alloy strengths, for reducing Magnesium Alloys Components cost, extend its application It is significant.Liquid nitrogen is the byproduct of oxygen industry processed, and source is wide, easily transport and storage, and cheap, chemical property is steady It is fixed, nontoxic pollution-free, do not corrode workpiece, carry out that subzero treatment is simple to operate, and cost is low with liquid nitrogen.Present invention is particularly directed to containing height The magnesium alloy of Al or high Sn elements, subzero treatment is carried out as processing medium using liquid nitrogen, and then improve magnesium alloy strength Purpose.
The content of the invention
The present invention is directed to during existing Magnesium Alloy Development, to improve Technology for Heating Processing or the use that intensity uses complexity Dilute noble alloy element such as rare earth element and cause corresponding parts cost too high so that be difficult to high-volume commercially produce should With the problem of, there is provided a kind of inexpensive, short cycle improves the processing method of magnesium alloy strength.This method passes through to magnesium alloy composition It is preferred, using cryogenic treatment process, the hardness of the system magnesium alloy can be significantly increased in a short time.This hair The bright magnesium alloy to high content Al or Sn has excellent treatment effect, so as to preferably meet industrial needs.
The technical scheme is that:
A kind of processing method for improving magnesium alloy strength, comprises the following steps:
1) as-cast magnesium alloy material is put into standing 5min~24h in liquid nitrogen, or as-cast magnesium alloy material is passed through successively It is put into after crossing solution treatment, plastic deformation processing in liquid nitrogen, stands 5min~24h;
Wherein, described magnesium alloy materials be containing 6~10%Al, 0.5~6%Sn, 0.5~2%Zn, or containing 6~ 10%Sn, 0.5~6%Al, 0.5~2%Zn, remaining is Mg and inevitable impurity;
2) magnesium alloy materials after subzero treatment are taken out, be placed in air, clear-cutting forestland to room temperature.
Described solution treatment comprises the following steps:Magnesium alloy materials are placed on to the heat-treatment furnace of argon gas atmosphere protection In, 4~24 hours are incubated at a temperature of 400~500 DEG C, is then taken out material from heat-treatment furnace, and be immediately placed in 35 Room temperature is cooled to after being quenched in~45 DEG C of warm water, i.e., solution treatment is carried out to material;
Described is plastic deformation to hot extrusion deformation, its crimp temperature be 200~350 DEG C, extrusion speed be 2~ 10m/min, extrusion ratio are 25~50.
The temperature of described liquid nitrogen is preferably -196 DEG C.
The magnesium alloy of special component by above-mentioned PROCESS FOR TREATMENT, hardness are greatly improved.
The present invention substantive distinguishing features be:
Described subzero treatment is currently only used for the common as cast condition commercialization magnesium alloy trade mark and the magnesium alloy system containing micro- rare earth, Purpose is concentrated mainly on the anti-wear performance that material is improved using cryogenic treatment process, due to the high-strength Mg-Sn based alloys of non-rare-earth type For the alloy system just developed in recent years, people study it not yet deep, are further carried especially by subzero treatment The research of its high comprehensive mechanical property has no report.So the present invention has been explored therein by largely studying and testing Certain law, and the zone of reasonableness of specific Sn, Al and Zn suitable for the technique are pointed out, demonstrate it has to wrought magnesium alloy Effect property.
When magnesium alloy materials carry out subzero treatment, because Quench causes Lattice Contraction, internal stress is generated in the sample, Cause stress concentration, induce and subgrain structure is produced in matrix and promotes solid solution element to be analysed in the form of the phase of nanoscale second Go out;When temperature changes, the volume of solid changes magnesium alloy materials, so as to produce stress and corresponding deformation in object Energy.When alloy is cooled to liquid nitrogen temperature from room temperature (about 25 DEG C) (about -196 DEG C), generated in alloy larger compression and Deformation energy, compression causes to produce a large amount of dislocations in alloy, and the deformation energy part in alloy is changed into heat, separately has quite A part is converted into interior energy, raises the interior energy of alloy, alloy structure is in metastable state, promotes a large amount of analysis of build up phase Go out, so that a large amount of second phase particles of carbides in the alloy;Subgrain structure in alloy greatly enhances with dislocation interaction The stability of structure;In addition, the effect of sub boundary is similar with crystal boundary, the motion of dislocation can be equally hindered, makes the power of material Performance is learned to be improved;After processing, a large amount of hardening constituents separated out in alloy play second-phase strength effect, further improve alloy Mechanical property.
Beneficial effects of the present invention are:
Generally conventional aging strengthening model is that sample is placed in heat-treatment furnace, unconspicuous especially for natrual ageing For magnesium alloy, for general artificial aging more using the 160-300 DEG C of temperature not waited, soaking time is more than 20 hours up to hundreds of small When, or hardness could be caused to peaking using multistage aging processing, consumed energy in whole ag(e)ing process more seriously, for complexity Parts even need several days;Meanwhile met constantly slightly along with the extension of aging time, the crystal grain of alloy and the second of precipitation Change and then drop low-alloyed performance.And the raw material liquid nitrogen wide material sources that subzero treatment uses, it is cheap.It is long-term preserve also compared with For convenience, volatile quantity is small and is easy to supplement, and is substantially not present power consumption, preserves can be long under the conditions of suitable sealing technology when.
The processing method of magnesium alloy described in patent of the present invention is compared with conventional solid solution processing and Ageing Treatment, technique letter Single, the process-cycle is short, easy to control, it is not necessary to complicated supporting equipment, the application being easy on related magnesium alloy material parts, It is adapted to high-volume commercial application;Subzero treatment can promote nano-second-phase disperse educt as conventional Ageing Treatment, but compared with Low temperature can effectively avoid crystal grain and Second Phase Particle from growing up, while the state is still kept not when alloy recovers to room temperature Become.The present invention can lift 30-50%, positive effect for the peak hardness after high Al and high Sn magnesium alloys subzero treatment.
Brief description of the drawings
Fig. 1 is the as cast condition TAZ711 of embodiment 1 hardness-deep cooling time graph
Fig. 2 is the As-extruded ATZ842 of embodiment 2 hardness-deep cooling time graph
Fig. 3 is the As-extruded AZ81 of embodiment 3 hardness-deep cooling time graph
Fig. 4 is the as cast condition ZK60 of comparative example 1 hardness-deep cooling time graph
Fig. 5 is the as cast condition of comparative example 2 and As-extruded AT31 hardness-deep cooling time graph
Fig. 6 is the as cast condition of comparative example 3 and As-extruded AZ31 hardness-deep cooling time graph
Embodiment
(technical scheme) of the invention is described further below by specific embodiments and the drawings, following examples are equal Implemented premised on technical solution of the present invention, give embodiment in detail and specifically operating process, but the present invention Protection domain be not limited to following embodiments.
A kind of inexpensive, short-period magnesium alloy processing method, this method can be directed to as-cast magnesium alloy and deformation states magnesium closes Gold carries out short time subzero treatment, greatly improves the hardness of alloy.
1) in the present invention, the magnesium alloy materials are preferably to contain 6~10%Al, 0.5~6%Sn, 0.5~2%Zn, remaining For Mg and inevitable impurity;Or containing 6~10%Sn, 0.5~6%Al, 0.5~2%Zn, remaining is for Mg and unavoidably Impurity.
2) the hot-working plastic deformations such as in the present invention, the deformation states refer to by extruding, rolling, drawing.Before plastic deformation Solution treatment need to be carried out to magnesium alloy:The magnesium alloy materials of above-mentioned special component are incubated at a temperature of 400~500 DEG C to 4~ 24 hours, then material is taken out from heat-treatment furnace, and be immediately placed in 35~45 DEG C of warm water and be cooled to room temperature.At solid solution Argon gas is passed through in the heating of reason and insulating process to be protected.
3) in the present invention, the subzero treatment includes, and using liquid nitrogen, with 1~10 DEG C/s cooling velocity, is opened from room temperature Begin, magnesium alloy materials are cooled to insulation 5min~24h under -196 DEG C of ultralow temperature.
4) in the present invention, magnesium alloy materials are placed in air clear-cutting forestland to room temperature after carrying out subzero treatment.
In order that the object, technical solutions and advantages of the present invention are clearer, the present invention is done below in conjunction with accompanying drawing into The displaying of one step.
Embodiment 1
According to the thinking of the present invention, design the low Al magnesium alloy materials TAZ711 of high Sn and carried out as sample at deep cooling reinforcing Reason, each predominant quantity percentage composition of the magnesium alloy is Sn:6.875%, Al:0.934%, Zn:0.892%, surplus is Mg and the micro inevitably impurity such as Mn, Si, Fe, Cu, Ni by being brought into when the pure magnesium of matrix and intermediate alloy melting.
Subzero treatment:As cast condition TAZ711 magnesium alloy samples are directly placed at the inner insulation 5min~12h of liquid nitrogen (- 196 DEG C), Clear-cutting forestland is then taken out to room temperature.
Micro-hardness testing:Using model MMT-X7 microhardness testers, to the magnesium alloy sample after subzero treatment Product carry out hardness test, and microhardness testers load selects 1kgf, dwell time 10s, show that m- hardness curve is as schemed during its deep cooling Shown in 1.
As seen from the figure, in subzero treatment, hardness gradually steps up as cast condition TAZ711 magnesium alloys with the extension of time, in deep cooling Processing reaches peak in 10 hours or so, hereafter begins to decline.Lifted from the 55Hv of initial as cast condition to 72Hv, improve 30%.
Embodiment 2
According to the thinking of the present invention, design and sample is used as by the low Sn magnesium alloy materials ATZ842 of high Al after crimp Product carry out deep cooling intensive treatment, and each predominant quantity percentage composition of the magnesium alloy is Al:8.312%, Sn:4.050%, Zn:1.862%, surplus be Mg and by brought into when the pure magnesium of matrix and intermediate alloy melting it is micro inevitably Mn, Si, Fe, The impurity such as Cu, Ni.
Subzero treatment;By As-extruded ATZ842 magnesium alloy samples be directly placed at the inner insulation 5min of liquid nitrogen (- 196 DEG C)~ 24h, clear-cutting forestland is then taken out to room temperature.
Performance detection is carried out to the magnesium alloy sample after subzero treatment, m- hardness curve such as Fig. 2 institutes during its deep cooling Show.
As seen from the figure, when As-extruded ATZ842 magnesium alloys are through subzero treatment, hardness significantly improves with the extension of time, Subzero treatment reaches peak in 2 hours, hereafter begins to decline.Lifted to Hv115, improved from the 90Hv of initial As-extruded 27.8%.
Embodiment 3
Deep cooling intensive treatment is carried out as sample using As-extruded commercialization AZ81 magnesium alloy materials, each composition of the magnesium alloy Weight percentage is Al:7.83%, Zn:0.921%, Sn:0.0032%, Mn:0.0091%, Si:0.0041%, Fe: 0.008%, Cu:0.0094%, Ni:0.0035%, surplus is Mg and inevitable impurity.
Subzero treatment;As-extruded AZ81 magnesium alloy samples are directly placed at the inner insulation 5min~24h of liquid nitrogen (- 196 DEG C), Clear-cutting forestland is then taken out to room temperature.
Performance detection is carried out to the magnesium alloy sample after subzero treatment, m- hardness curve such as Fig. 3 institutes during its deep cooling Show.
As seen from the figure, when As-extruded AZ81 magnesium alloys are through subzero treatment, with the extension hardness elder generation rapid increase of soak time After decline and rise again, reach peak within 2 hours in subzero treatment.Lifted to 105Hv, improved from the 70Hv of initial As-extruded 50%.
Comparative example 1
Using as cast condition commercialization ZK60 magnesium alloy materials deep cooling intensive treatment, the weight of each composition of the magnesium alloy are carried out as sample Amount percentage composition is Zn:6.13%, Zr:0.221%, Mn:0.0079%, Si:0.0063%, Fe:0.006%, Cu: 0.0088%, Ni:0.0051%, surplus is Mg and inevitable impurity.
Subzero treatment;ZK 60 Magnesium Alloy sample is directly placed at the inner insulation 5min~12h of liquid nitrogen (- 196 DEG C), so Clear-cutting forestland is taken out afterwards to room temperature.
Performance detection is carried out to the magnesium alloy sample after subzero treatment, m- hardness curve such as Fig. 4 institutes during its deep cooling Show.
As seen from the figure, ZK 60 Magnesium Alloy is presented with the extension hardness of time and fluctuated up and down in subzero treatment, processing Front and rear firmness change is little, i.e. high Zn content magnesium alloy is insensitive to subzero treatment, DeGrain.
Comparative example 2
According to the thinking of the present invention, design as cast condition and the low Sn magnesium alloy materials AT31 of the low Al of As-extruded and carried out as sample Deep cooling intensive treatment, each predominant quantity percentage composition of the magnesium alloy are Al:2.852%, Sn:0.781%, surplus Mg And the micro inevitably impurity such as Zn, Mn, Si, Fe, Cu, Ni by being brought into when the pure magnesium of matrix and intermediate alloy melting.
Subzero treatment;As cast condition and As-extruded AT31 magnesium alloy samples is directly placed to liquid nitrogen (- 196 DEG C) is inner to be incubated respectively 5min~12h, clear-cutting forestland is then taken out to room temperature.
Performance detection is carried out to the magnesium alloy sample after subzero treatment, it is m- when as cast condition and its deep cooling of As-extruded sample Hardness curve is as shown in Figure 5.
As seen from the figure, as cast condition and As-extruded AT31 magnesium alloys are presented in subzero treatment with the extension hardness of time Lower fluctuation, firmness change is little before and after the processing, i.e. the low Sn contents magnesium alloys of the low Al of as cast condition and deformation states are insensitive to subzero treatment, DeGrain.
Comparative example 3
Deep cooling intensive treatment is carried out as sample using as cast condition and As-extruded commercialization AZ31 magnesium alloy materials, the magnesium alloy is each The weight percentage of composition is Al:3.18%, Zn:0.85%, Mn:0.335%, Si:0.02%, Fe:0.005%, Cu: 0.05%, Ca:0.04%, surplus is Mg and inevitable impurity.
Subzero treatment;As cast condition and As-extruded AZ31 magnesium alloy samples is directly placed to liquid nitrogen (- 196 DEG C) is inner to be incubated 5min ~12h, clear-cutting forestland is then taken out to room temperature.
Performance detection is carried out to the magnesium alloy sample after subzero treatment, it is m- when as cast condition and its deep cooling of As-extruded sample Hardness curve is as shown in Figure 6.
As seen from the figure, as cast condition and As-extruded AZ31 magnesium alloys are presented in subzero treatment with the extension hardness of time Lower fluctuation, firmness change is little before and after the processing, i.e., low Al is low, and Zn contents magnesium alloy is insensitive to subzero treatment, DeGrain.
By above example as can be seen that the height of specific alloy elements content and subzero treatment effect in magnesium alloy Contact is closely.Subzero treatment is to the high Al of the high Sn low Al or low Sn Mg-Sn-Al alloys that filter out and the low Zn of high Al Mg-Al-Zn alloys influence that significantly, its microhardness can be significantly improved;But for the low Sn of low Al, low Al low Zn, high Zn content For magnesium alloy, it is less sensitive to subzero treatment, DeGrain.I.e. subzero treatment be directed to patent of the present invention in it is specific into Divide magnesium alloy system to have and preferably strengthen effect, newly think to improve the intensity of this novel high-strength heat resistance magnesium alloy and providing to strengthen Road and technical strategies.
The above embodiment of the present invention is only example to illustrate the invention, and is not the implementation to the present invention The restriction of mode.For those of ordinary skill in the field, other can also be made not on the basis of the above description With the change and variation of form.Here all embodiments can not be exhaustive.It is every to belong to technical scheme Row of the obvious changes or variations amplified out still in protection scope of the present invention.
Unaccomplished matter of the present invention is known technology.

Claims (4)

  1. A kind of 1. processing method for improving magnesium alloy strength, it is characterized in that this method comprises the following steps:
    1)As-cast magnesium alloy material is put into standing 5min ~ 24h in liquid nitrogen, or by as-cast magnesium alloy material successively by being dissolved It is put into after processing, plastic deformation processing in liquid nitrogen, stands 5min ~ 24h;
    Wherein, described magnesium alloy materials are containing 6 ~ 10%Al, 0.5 ~ 6%Sn, 0.5 ~ 2%Zn, or containing 6 ~ 10%Sn, 0.5 ~ 6% Al, 0.5 ~ 2%Zn, remaining is Mg and inevitable impurity;
    2)Magnesium alloy materials after subzero treatment are taken out, are placed in air, clear-cutting forestland to room temperature.
  2. 2. as claimed in claim 1 improve magnesium alloy strength processing method, it is characterized in that described solution treatment include with Lower step:Magnesium alloy materials are placed in the heat-treatment furnace of argon gas atmosphere protection, 4 ~ 24 are incubated at a temperature of 400 ~ 500 DEG C Hour, then material is taken out from heat-treatment furnace, and be immediately placed in quenched in 35 ~ 45 DEG C of warm water after be cooled to room Temperature, that is, complete to carry out solution treatment to material.
  3. 3. the processing method of magnesium alloy strength is improved as claimed in claim 1, it is characterized in that described is plastic deformation to hot extrusion Compressive strain, its crimp temperature are 200 ~ 350 DEG C, and extrusion speed is 2 ~ 10m/min, and extrusion ratio is 25 ~ 50.
  4. 4. the processing method of magnesium alloy strength is improved as claimed in claim 1, it is characterized in that the temperature of described liquid nitrogen is preferred For -196 DEG C.
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CN109735746A (en) * 2019-03-01 2019-05-10 吉林大学 A kind of raising aluminum alloy heat stability and superplastic preparation method
CN109837437A (en) * 2019-02-27 2019-06-04 吉林大学 A kind of alternating temperature controlled rolling preparation method for making low content magnesium alloy that there is uniform fine grain
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CN112680587A (en) * 2020-11-12 2021-04-20 淮阴工学院 Method for improving hardness of aluminum-magnesium alloy welding wire
CN113600629A (en) * 2021-08-09 2021-11-05 西北工业大学 Capillary tube deep cold drawing device and drawing method

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CN109622648A (en) * 2019-01-10 2019-04-16 吉林大学 A kind of magnesium alloy asymmetric continuous large deformation extrusion process forming method
CN109622649A (en) * 2019-01-10 2019-04-16 吉林大学 A kind of magnesium alloy continuous variable cross section large deformation extrusion process forming method
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CN109735746A (en) * 2019-03-01 2019-05-10 吉林大学 A kind of raising aluminum alloy heat stability and superplastic preparation method
CN110284033A (en) * 2019-08-05 2019-09-27 深圳市爱斯特新材料科技有限公司 A kind of Mg-Zn-Al base microalloying magnesium alloy of high intensity and preparation method thereof
CN110284033B (en) * 2019-08-05 2020-11-24 深圳市爱斯特新材料科技有限公司 High-strength Mg-Zn-Al-based microalloyed magnesium alloy and preparation method thereof
CN112680587A (en) * 2020-11-12 2021-04-20 淮阴工学院 Method for improving hardness of aluminum-magnesium alloy welding wire
CN113600629A (en) * 2021-08-09 2021-11-05 西北工业大学 Capillary tube deep cold drawing device and drawing method

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