CN110257678A - A kind of high-intensity thermal deformation resistant magnesium alloy material and preparation method thereof - Google Patents

A kind of high-intensity thermal deformation resistant magnesium alloy material and preparation method thereof Download PDF

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CN110257678A
CN110257678A CN201910689257.5A CN201910689257A CN110257678A CN 110257678 A CN110257678 A CN 110257678A CN 201910689257 A CN201910689257 A CN 201910689257A CN 110257678 A CN110257678 A CN 110257678A
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magnesium alloy
alloy
magnesium
thermal deformation
temperature
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CN110257678B (en
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齐福刚
叶芝松
侯彩红
李连辉
叶雪
曹红帅
赵镍
刘应都
欧阳晓平
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Xiangtan University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/002—Changing 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon

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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Extrusion Of Metal (AREA)
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Abstract

The invention discloses a kind of high-intensity thermal deformation resistant magnesium alloy materials, which is characterized in that its component includes: 5~7.15wt.%Zn, 4.1~6wt.%Sn, 0.6~2.2wt.%Mn, 0.2~0.8wt.%Al, inevitable impurity≤0.15%, surplus Mg.The invention also discloses the preparation methods of the high-intensity thermal deformation resistant magnesium alloy material, it is characterised in that: including (1) melting；(2) it machines；(3) Homogenization Treatments；(4) hot extrusion.Mg-Zn-Sn-Mn-Al alloy extrudate tensile strength prepared by the present invention is up to 422Mpa, and yield strength is up to 372Mpa, and furthermore 150 DEG C of average elongations of As-extruded are up to 65% or more.Therefore the present invention has good application and promotion prospect, can apply in the inexpensive civil field such as electric motor coach, rail traffic.

Description

A kind of high-intensity thermal deformation resistant magnesium alloy material and preparation method thereof
Technical field
The present invention relates to magnesium alloy production field in non-ferrous metal, it is related to a kind of the high-strength of room temperature high-strength high-temperature high-ductility Heat-resistant deforming magnesium alloy
Background technique
Compared to other structural materials, magnesium alloy has density low, and light weight, antidamping vibratility is strong, and casting character is excellent More, the advantages that machinability is good, and dimensional stability is high, and electromagnetic shielding capability is strong, and recovery utilization rate is high, therefore magnesium alloy is wide It is general to be applied to the fields such as automobile, electronics, electric appliance, traffic, space flight, aviation and defense military industry.But the exploitation journey of magnesium alloy Spend it is also much relatively low, annual output only has the 1% of aluminium alloy, be far from giving full play to its potential advantages, mainly due to Following reason: the absolute intensity of magnesium alloy is lower, and heat resistance is poor；Most of magnesium structural member both is from a kind of processing of die casting Mode, i.e. cast magnesium alloy.Since cast magnesium alloy morphotropism is poor, complex load cannot be born and volume is relatively small, magnesium The use of alloy is more limited.Compared with cast magnesium alloy, wrought magnesium alloy has excellent comprehensive mechanical property, higher Intensity and plasticity, more suitable for production large-sized structural parts and meet structure diversification requirement, therefore it is heat-resisting to develop novel high-strength Wrought magnesium alloy has important current demand and strategic importance.
Currently, on the one hand common commercial wrought magnesium alloy has that AZ is serial, such as AZ31 series deformation magnesium alloy, but its room temperature is anti- Tensile strength is lower than 260Mpa, and yield strength is lower than 200Mpa, and 150 DEG C of high temperature elongation percentage are lower than 25%, it is therefore apparent that AZ system magnesium closes The mechanical property of gold is also much unable to satisfy present civilian demand.
On the other hand, inventor once researched and developed the rare-earth-contained magnesium alloy of higher performance, and applied for related patents, such as The magnesium-zinc-manganese of CN201110005905- high zinc content-cerium system magnesium alloy materials；With a kind of high intensity of CN201110150964- Magnesium-zinc-manganese-yttrium-magnesium alloy material and a kind of high-intensitive magnesium-zinc-manganese-yttrium-cerium-magnesium alloy of CN201611248843- and its system Preparation Method.These magnesium-rare earth performances are higher, but due to causing cost of alloy higher containing rare earth, therefore be not suitable for existing extensively Civil field is promoted.
Inventor's early-stage study discovery, even if not using rare earth element, by alloying appropriate, with Mg-Zn system alloy Based on, along with the ageing strengthenings elements such as Sn and Al can also improve the synthesis of magnesium alloy by adjusting element quality proportioning Mechanical property greatly promotes the mechanical property of low-cost magnesium alloy, reaches the mechanics effect of similar rare earth alloy, will make The application of magnesium alloy is further promoted.
Therefore one kind how is designed not using rare earth element, Zn, Al, Sn, the more cheap element such as Mn are only selected, and pass through and close There is room temperature high-strength high-temperature high-ductility, the high-intensity thermal deformation resistant magnesium that mechanical property greatly promotes closes after suitable heat treatment process Gold, becoming has the technical issues of considered solution.
Summary of the invention
In view of the above shortcomings of the prior art, it is not used the technical problems to be solved by the present invention are: how to provide one kind Rare earth element only selects Zn, Al, Sn, the more cheap element such as Mn, but still has room temperature high-strength high-temperature high-ductility, mechanical property High-intensity thermal deformation resistant magnesium alloy material that can be greatly promoted and preparation method thereof can be effectively improved the tissue of alloy, carefully Change crystal grain；Being formed has the second phase fine and close, that fusing point is high, thermal stability is good, obtains the room temperature of alloy and mechanical behavior under high temperature Improve.
In order to solve the above-mentioned technical problem, present invention employs the following technical solutions:
A kind of high-intensity thermal deformation resistant magnesium alloy of room temperature high-strength high-temperature high-ductility, by mass percentage, the magnesium close Gold is composed of the following components: 5~7.15wt.%Zn, 4.1~6wt.%Sn, 0.6~2.2wt.%Mn, 0.2~0.8wt.% Al, inevitable impurity≤0.15%, surplus Mg.
This element matches the cast sturcture that can effectively improve alloy, refines crystal grain, and is conducive to generate high-melting-point Mg2Sn Phase, high-melting-point MnSn2Phase, high-melting-point Al-Mn phase and new high-melting-point Mg32(Al,Zn)49Ternary phase.According to the mix proportion scheme The Mg-Zn-Sn-Mn-Al alloy extrudate of preparation is according to theoretical direction and actual experimental check, by suitable timeliness heat After processing, tensile strength is up to 422Mpa, and yield strength is up to 372Mpa, and furthermore 150 DEG C of average elongations of As-extruded are reachable 65% or more.Therefore, alloy of the invention and corresponding preparation method have good application and promotion prospect, can be electronic It is applied in the low cost civil field such as car, rail traffic.And since this alloy has extremely excellent extension at high temperature Rate is very suitable to be processed into the higher part of precision and be fabricated under high temperature to need the impact-resistant components of damping.
Preferably, by mass percentage, the magnesium alloy is composed of the following components: Zn:5~6wt.%, Sn:4.1~ 5wt.%, Mn:0.6~1.5wt.%, Al:0.5~0.8wt.%, inevitable impurity≤0.15%, surplus are magnesium.
In proportional region after optimizing in this way, alloy property is more excellent.
Preferably, by mass percentage, the magnesium alloy is composed of the following components: Zn:5.9wt.%, Sn: 4.1wt.%, Mn:0.9wt.%, Al:0.6wt.%, inevitable impurity≤0.15%, surplus are magnesium.
The preferred proportion enables to magnesium alloy to have more excellent performance, has room temperature more outstanding high-intensitive high Warm high-ductility feature.
The invention also discloses the preparation methods of above-mentioned high-intensity thermal deformation resistant magnesium alloy, comprising the following steps:
(1) melting: with pure Mg, pure Zn, pure Sn, pure Al, Mg-10wt.%Mn are raw material, by the matter of the magnesium alloy component Amount percentage carries out calculating ingredient, and the pure magnesium ingot for being preheating to 150 ± 5 DEG C is added in resistance furnace, heats to 720 ± 5 DEG C It melts to obtain Serum Magnesium to the pure magnesium ingot, by Serum Magnesium temperature control successively by remaining alloy raw material after 720 ± 5 DEG C The Serum Magnesium is added to abundant fusing, refining agent refining stirring fishing slag is added, be warming up to 740 DEG C of ± 5 DEG C of heat preservations 35~ 45min, slag hitting is stirred after standing again, keeps the temperature 10~20min, finally uses die cast, and magnesium alloy ingot is made；Entirely Fusion process is in CO2And SF6Mixed gas protected lower progress；
(2) it machines: the oxide skin on magnesium alloy ingot surface in removal step (1), and by ladle barrow at diameter 80mm；
(3) Homogenization Treatments: the ingot casting after peeling is warming up to 310 DEG C~340 DEG C, keeps the temperature 14~16 hours, then again It is secondary to be warming up to 360 DEG C~380 DEG C, 2~3 hours are kept the temperature, is finally warming up to 400 DEG C~420 DEG C, 2~3 hours is kept the temperature, is air-cooled to Room temperature；
(4) hot extrusion: will be 25:1 in extrusion ratio through step (3) treated magnesium alloy ingot, extrusion speed is 1~ 3mm/s carries out hot extrusion under the conditions of 330~360 DEG C.
On the basis of determining alloying element mass ratio, suitable heat treatment method can increase substantially the resultant force of alloy Learn performance.Using above-mentioned heat treatment method, it can reliably make the performance of alloy material get a promotion, make its tensile strength can Up to 422Mpa, yield strength is up to 372Mpa, and furthermore 150 DEG C of average elongations of As-extruded are up to 65% or more.
In view of this alloy is Mg-Zn system alloy, along with ageing strengthenings element, this alloy such as Sn and Al have huge Ageing strengthening potentiality.Therefore, further, wherein the heat treatment process of extruded bars are as follows:
1) solution treatment+single-stage aging processing (T6)；
I.e. first 400~440 DEG C solution treatment 1~6 hour, water quenching to room temperature；Then at 140~260 DEG C timeliness 6~ 24 hours, it is air-cooled to room temperature.
General aging temp is lower, and the time used in arrival peak timeliness is longer, and alloy comprehensive mechanical property is better, conversely, Aging temp is higher, and the time used in arrival peak timeliness is shorter, and alloy comprehensive mechanical property is relatively low.But compare two-stage time effect For, this heat treatment method time-consuming is shorter, so this heat treatment method is more suitable for needing to save the civil field of time cost.
Alternatively, the heat treatment process of extruded bars can be with are as follows:
2) solution treatment+two-stage time effect processing (T4+Two step-aging)；
I.e. first 400~440 DEG C solution treatment 1~6 hour, water quenching to room temperature；Then the timeliness for the first time at 70~90 DEG C 16~24 hours, then timeliness 6~24 hours at 140~260 DEG C, were air-cooled to room temperature.
Since aging temp selection is lower, longer the time required to reaching peak timeliness, alloy comprehensive mechanical property is higher, instead It, aging temp is higher, and the time used in arrival peak timeliness is shorter, and alloy comprehensive mechanical property is relatively low.But two-stage time effect Comprehensive mechanical property is more superior compared to single-stage aging, therefore is more suitable for disregarding the defense industry of cost and space flight and aviation neck Domain.
Preferably, in step (1), the die cast is to be poured into Serum Magnesium to be preheating to 600 ± 5 DEG C of cast iron casting mould In.
After optimizing in this way, can alloy solution more slowly be cooled down, so that timely feeding, finally closes as cast condition Gold reduces the casting flaws such as Shrinkage cavity.
Preferably, in step (1), the CO2And SF6Mixed gas in SF6Shared volume fraction is 0.01%.
In this way optimize after, alloy solution and oxygen-barrier can be made, thus inhibit alloy melting vigorous oxidation and It is fire-retardant, SF6Protection philosophy is 2Mg+O2=2MgO
2Mg+O2+SF6=2MgF2+SO2F2
2MgO+SF6=2MgF2+SO2F2
SF6It is related with its content to the anti-flaming protective effect of magnesium liquid.The SF in mixed gas6Volume fraction reach 0.01% is just enough to form good protective film on magnesium liquid surface.Volume fraction is too small, then MgF2Production quantity is few, and skin covering of the surface is inadequate It is fine and close；If SF6Volume fraction it is excessive, then MgF2Production quantity is excessive, and film thickens embrittlement, is also easy to produce crackle, makes protective effect instead Weaken, while also there is serious corrosiveness to equipment.
Its CO2Protection philosophy is 2Mg+CO2=2MgO+C
4Mg+CO2=Mg2C+2MgO
Above-mentioned reaction, which is formed by film and is able to suppress magnesium liquid, to be continued to aoxidize, and is because occurring in oxidation film unformed Carbon, this unformed carbon be uniformly distributed in oxidation intermembrane space in, improve the consistency of oxidation film, reach consistency coefficient To 1.03~1.15.
Preferably, in step (3), the Homogenization Treatments specifically: the ingot casting after peeling is warming up to 310 DEG C~340 DEG C, keep the temperature 14~16 hours, be then warming up to 360 DEG C~380 DEG C again, keep the temperature 2~3 hours, be finally warming up to 400 DEG C~ 420 DEG C, 2~3 hours are kept the temperature, room temperature is air-cooled to.
Using the homogenizing processing mode of above-mentioned optimization, can component segregation be improved, classification homogenization can have Effect prevention alloy causes local temperature excessively high due to being rapidly heated so as to cause generation the case where alloy burning, and then after being conducive to Continuous extruding.
Preferably, in step (4), the hot extrusion specifically: extrusion ratio be 25:1, extrusion speed be 1~3mm/s, Hot extrusion is carried out under the conditions of 330~360 DEG C.
Using above-mentioned squeezing parameter, As-extruded alloy can be made to possess good reinforcing phase size and tiny crystalline substance Grain.As shown in figure 9, crystallite dimension substantially at 5 μm, is largely strengthened, phase size is dispersed and tiny to be distributed in transgranular and crystal boundary, thus So that As-extruded alloy possesses good comprehensive mechanical property.Extrusion ratio is the most obvious to the Effect on Mechanical Properties of alloy, squeezes The degree of difficulty of metal outflow die hole will increase while than increasing, and extruding force also increases, and excessive extrusion ratio is easy so that squeezing Press alloy crack.Crystal grain can reduce while extrusion ratio reduces, and strengthening phase size will increase, and too small extrusion ratio can be up to not To the best comprehensive mechanical property of alloy.
The principle of the present invention and design philosophy is described below are as follows:
(1) present invention selects the elements such as lower-cost Zn, Sn, Mn, Al, by adjusting element mass ratio, it is intended to can obtain A kind of it can must partially replace novel wrought magnesium alloy of the high cost containing rare earth element.The present invention uses Zn for the first component.Zn member The addition of element can be improved alloy flowability, so as to improve the casting character of alloy, but excessively high Zn content will cause it is serious Hot tearing and shrinkage porosite；And it is lower than the Zn content of this range, it will cause main hardening constituent Mg32(Al,Zn)49Quantity is reduced, simultaneously because Zn/Al mass ratio reduces, the Mg of thermal stability difference17Al12Quantity will increase, so as to cause alloy comprehensive mechanical property decline, Therefore best Zn content range is 5~7.15wt.%.It, can be with from mechanical property table in addition, this is theoretical for 12 susceptible of proof of embodiment Find out, Zn/Al mass ratio, which reduces, influences significantly comprehensive mechanical property.In addition, because when Zn has very strong in the magnesium alloy Precipitation strength effect is imitated, so Mg-Zn system alloy is heat-treatable alloy system.
(2) present invention uses Sn for the second component.Studies have shown that Mg-Zn system alloy high-temp performance is short of, but Sn element Addition theoretically can be generated hard resistant to high temperature and stablize the second phase Mg2Sn, to improve the mechanical behavior under high temperature of alloy, furthermore Can also effectively inhibit magnesium alloy component segregation and due to Zn element bring hot cracking tendency etc. adversely affect, but its second Mutually it is brittlement phase, plasticity can be reduced, therefore Sn content optimal components are 4.1~6wt.%.When Sn content is too low, High-Temperature Strengthening Phase Mg2Sn is reduced, comprehensive mechanical property decline.13 comprehensive mechanical property susceptible of proof of embodiment.
(3) present invention uses Mn for third component.A small amount of Mn element can settle impurity element during melting and casting, So that alloy corrosion resistance is promoted.Because the second constituent element has selected Sn element, alloy corrosion resistance reduction will lead to, so one A small amount of Mn element, which is added, in aspect can effectively improve alloy corrosion resistance, and Sn element bring adverse effect is added to alleviate.It is another Fermentation can also form the second phase of high temperature resistant MnSn with Sn element2But if Mn too high levels, tiny disperse MnSn2It will become Must be coarse, it causes stress to concentrate, easily becomes formation of crack, and Mn will be converted into2Lower melting-point coarse second phase such as Sn. If Mn content is too low simultaneously, main High-Temperature Strengthening phase MnSn2And Al-Mn phase is difficult to generate, so that the room temperature of alloy It is reduced with high temperature comprehensive mechanical property, therefore Mn optimum content is 0.6~2.2wt.%.
(4) present invention uses Al for the 4th component.By adjusting Zn/Al mass ratio, thermostabilization theoretically not only can avoid Property difference Mg17Al12It generates, and new high-melting-point can be generated and stablize ternary phase Mg32(Al,Zn)49, and with the 4th constituent element Mn Element generation it is new stablize heat-resisting second phase Al8Mn5And Al3Mn, so with high-temperature stable phase Mg2Sn collective effect, to height Grain Boundary Sliding and dislocation motion under temperature play pinning effect, to further increase the mechanical behavior under high temperature of alloy, furthermore Al The addition of element can produce stronger ageing strengthening effect to improve Alloy At Room Temperature, elevated temperature strength and improve alloy castability Can, therefore Al optimum content is 0.2~0.8wt%.In the present solution, the ratio of Al is unsuitable excessively high, if excessively high, will affect Mg and The combination of Sn, significantly reduces alloy property.
(5) after alloy each element mass ratio is decided.The heat treatment process of extruded bars becomes particularly important, according to member Mass ratio between element, and Mg-Zn, Mg-Al isofacies map and pertinent literature are referred to, determine best solid solubility temperature 400~440 DEG C, the time is 1~6 hour, and solution treatment main purpose makes to close exactly in order to make divorsed eutectic phase, transgranular second phase decomposition Each element diffuses into α-Mg matrix in gold, forms supersaturated solid solution, and solution treatment is usually in magnesium alloy heat treatment Between process, need to make next step Precipitation heat treatment.In other words, if grown up and in burning or excessive grain Without being dissolved substantially, optimum efficiency will be not achieved in subsequent ageing treatment for two-phase.
(6) ageing treatment is carried out after solution treatment, dispersed and tiny precipitated phase can be precipitated from supersaturated solid solution, although There is also these phases in as-cast structure, but are often present on crystal boundary in the form of coarse divorsed eutectic, make to material property At adverse effect.If habit plane, shape, size and the distribution of hardening constituent can be changed by deformation, aging strengthening model, from And make to strengthen the ability enhancing for hindering dislocation movement by slip and pinning crystal boundary, so that it may significantly improve the room temperature and high-temperature mechanics of alloy Energy.Learning Mg-Zn system alloy, there are preageing precipitate phases, will form the area G.P. at 110 DEG C or less, can be subsequent high temperature Timeliness provides a large amount of nucleation mass point, so as to increase substantially the comprehensive mechanical property of alloy.But this alloy system because More for element, the formation temperature in the area G.P. can change, and according to experimental result, this alloy is in 70~90 DEG C of discovery G.P. Area, therefore, the confirmable temperature range of preageing in two-stage time effect at 70~90 DEG C, time range 16~for 24 hours.For rear Continuous single-stage aging and second level aging technique determine, because if heating temperature is excessively high or soaking time is too long, can generate Timeliness and reduce mechanical property, therefore, optimal aging treatment process and spy can be made by age hardening curves The relationship between aging temp and time is studied carefully, to achieve the purpose that obtain optimal heat treatment process with the smallest cost.
Compared with prior art, the beneficial effects of the invention are as follows (since the benefit performance of alloy usually needs verification experimental verification, So explanation is introduced in test data and attached drawing in introduction combination subsequent embodiment):
(1) present invention has chosen Zn as main alloy element, i.e. this alloy system is the Mg- for possessing ageing strengthening potentiality Zn system alloy.According to experimental result, on the one hand, ingot casting obtained by the melting of this alloy system is all right, and obtained by subsequent extrusion Alloy bar material surface does not occur the defects of a large amount of crackles, on the other hand, comprehensive mechanical property after this alloy is heat-treated as known from Table 2 It is substantially improved.
(2) present invention uses Sn for the second component, from the XRD in Fig. 1 it is found that alloy generates hard stabilization resistant to high temperature Second phase Mg2Sn, this alloy high-temp excellent in mechanical performance, improves most of Mg-Zn system alloy high-temp mechanical property as known from Table 2 The status that energy is not good enough, and four AZ91 of contrast table etc. is free of Sn mischmetal, and this alloy system mechanical behavior under high temperature significantly mentions Height, wherein high-temperature stable phase Mg2Sn plays an important role.
(3) present invention uses Mn for third component, from the XRD in Fig. 1 it is found that because having chosen suitable Mn content, closes Gold generates dispersed and tiny MnSn2The second phase of high temperature resistant, as known from Table 2, the mechanical behavior under high temperature of embodiment 6 compare embodiment 4 and 5 is slightly weak, is because embodiment 6 has lacked dispersed and tiny MnSn2, so superior mechanical behavior under high temperature and MnSn2Have close Inseparable connection.
(4) present invention uses Al for the 4th component, from the XRD in Fig. 1 it is found that this alloy system to avoid thermal stability poor Mg17Al12, generate heat-resistant stable ternary phase Mg32(Al,Zn)49And the new Al of Mn Element generation8Mn5And Al3Mn。 In addition, from the DSC in Fig. 6 it is found that the increase of Al content is so that melting the temperature at peak reduces, therefore the addition of Al to close really The casting character of gold is improved.State institute finally, tying, contrast table 3 and table 4 it is found that this alloy system ambient temperature mechanical properties and Mechanical property is promoted obvious after heat treatment.Obviously, be between different elements it is interactional, element ratio difference obtain second It is mutually also different, and then largely effect on alloy mechanical property.In addition, can be obtained from embodiment 10 and embodiment 11, Zn/Al mass ratio It is unsuitable excessively high, otherwise by the comprehensive mechanical property of extreme influence alloy.
(5) solution treatment is carried out to extruded bars, according to Fig. 4 and Fig. 5 it is found that in the range of optimum temperature and time, Grain size is uniformly and the second phase of bulk is dissolved substantially into matrix, is conducive to subsequent aging strengthening model.
(6) ageing treatment is carried out after solid solution, according to the age hardening curves in Fig. 7 and 8 it is found that preageing stage, shape At the area G.P., nucleation mass point is improved for subsequent precipitated phase, there is no too big variations for hardness.In the lack time effect stage, hardness is compared to pre- Timeliness increases considerably, and rate of rise reaches peak value, and rate of rise slows down later, this is primarily due in this alloy system Small and dispersed Mg2Sn phase, high-melting-point MnSn2Phase, high-melting-point Al-Mn phase and high-melting-point Mg32(Al,Zn)49The body of ternary phase Fraction precipitation rate significantly increases compared to preageing, and precipitate volume fraction growth slows down after lack time effect.The peak timeliness stage, Hardness reaches maximum, this precipitate volume fraction for being primarily due to small and dispersed in this alloy system reaches maximum, right at this time The time answered is also the best heat treatment time of aging heat treatment.Overaging stage, hardness slowly reduce, this is primarily due to this Precipitate size appearance in alloy system, which is generally grown up, to be caused.According to the different age hardening curves of Fig. 7 and Fig. 8, can obtain Know that the time used in arrival peak timeliness is longer, but hardness is higher when aging temp is lower, conversely, reaching peak when aging temp is about high Time used in timeliness is shorter, but hardness is lower.In conclusion best single-stage aging temperature and second level aging range determine At 150~180 DEG C, aging time 20~for 24 hours.Best aging treatment process has been made according to age hardening curves, has been reached With the smallest cost obtain the purpose of optimal heat treatment process.According to table 2, the alloy mechanical property after ageing treatment is compared As-extruded, tensile strength and yield strength increase substantially, and elongation percentage is declined slightly, and two-stage time effect treated resultant force It is more superior than single-stage aging to learn performance.Illustrate that age hardening curves have important references meaning for formulating optimum treatment process Justice.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out Illustrate:
Fig. 1 is the X-ray diffractogram of the Mg-Zn-Sn-Mn-Al series deformation magnesium alloy prepared in embodiment 4~6.
Fig. 2 is fracture after 150 DEG C of As-extruded of the Mg-Zn-Sn-Mn-Al series deformation magnesium alloy prepared in embodiment 5 stretch Secondary electron scanning electron microscope.
Fig. 3 is fracture after 150 DEG C of As-extruded of the Mg-Zn-Sn-Mn-Al series deformation magnesium alloy prepared in embodiment 5 stretch Back scattering scanning electron microscope.
Fig. 4 is the solid solution state microstructure metallographic of the Mg-Zn-Sn-Mn-Al series deformation magnesium alloy of middle preparation in embodiment 5 Figure.
Fig. 5 is the solid solution state microstructure SEM of the Mg-Zn-Sn-Mn-Al series deformation magnesium alloy prepared in embodiment 5.
Fig. 6 is the differential thermal analysis of the Mg-Zn-Sn-Mn-Al series deformation magnesium alloy prepared in embodiment 4~6.
Fig. 7 be Mg-Zn-Sn-Mn-Al series deformation magnesium alloy single-stage aging at different temperatures prepared by embodiment 5 and The age hardening curves of two-stage time effect.
Fig. 8 is the single-stage aging and two-stage time effect of the Mg-Zn-Sn-Mn-Al series deformation magnesium alloy prepared in embodiment 4~6 Age hardening curves.
Fig. 9 is the As-extruded longitudinal section microstructure of Mg-Zn-Sn-Mn-Al series deformation magnesium alloy prepared by embodiment 5 SEM。
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments.
Below by a preferred embodiment of the present invention will be described in detail
Embodiment
Table 1 is the constituent mass percent of each Mg-Zn-Sn-Mn-Al wrought magnesium alloy in 14 groups of embodiments.
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
Including in above-mentioned 14 embodiments, the high-intensity thermal deformation resistant magnesium of any room temperature high-strength high-temperature high-ductility is closed Gold, when preparation include being divided into melting, are squeezed and the stages such as heat treatment process；
(1) melting: with pure Mg, pure Zn, pure Sn, pure Al, Mg-10wt.%Mn are raw material, by the matter of the magnesium alloy component Amount percentage carries out calculating ingredient, and the pure magnesium ingot for being preheating to 150 ± 5 DEG C is added in resistance furnace, heats to 720 ± 5 DEG C It is melted to the pure magnesium ingot, after 720 ± 5 DEG C successively the magnesium is added in the intermediate alloy by Serum Magnesium temperature control Melt is added refining agent refining stirring fishing slag, is warming up to 740 DEG C of ± 5 DEG C of 35~45min of heat preservation, stands again to abundant fusing Slag hitting is stirred afterwards, keeps the temperature 10~20min, finally uses die cast, and magnesium alloy ingot is made；Entire fusion process is in CO2 And SF6Mixed gas protected lower progress；Wherein, volume fraction shared by SF6 is 0.01% in mixed gas.
(2) it machines: the oxide skin on magnesium alloy ingot surface in removal step (1), and by ladle barrow at diameter 80mm；
(3) Homogenization Treatments: the ingot casting after peeling is warming up to 310 DEG C~340 DEG C, keeps the temperature 14~16 hours, then again It is secondary to be warming up to 360 DEG C~380 DEG C, 2~3 hours are kept the temperature, is finally warming up to 400 DEG C~420 DEG C, 2~3 hours is kept the temperature, is air-cooled to Room temperature.
(4) hot extrusion: will be 25:1 in extrusion ratio through step (3) treated magnesium alloy ingot, extrusion speed is 1~ 3mm/s carries out hot extrusion under the conditions of 330~360 DEG C.
Wherein, the heat treatment process of extruded bars has following two:
1) solution treatment+single-stage aging (T6)；
First 400~440 DEG C solution treatment 1~6 hour, water quenching to room temperature；Then the timeliness 6~24 at 140~260 DEG C Hour, it is air-cooled to room temperature；Aging temp is lower, and the time used in arrival peak timeliness is longer, and alloy comprehensive mechanical property is better, instead It, aging temp is higher, and the time used in arrival peak timeliness is shorter, and alloy comprehensive mechanical property is relatively low.But compare twin-stage For timeliness, this heat treatment method time-consuming is shorter, so this heat treatment method is more suitable for needing to save the civilian of time cost Field.
2) solution treatment+two-stage time effect (T4+Two step-aging)；
First 400~440 DEG C solution treatment 1~6 hour, water quenching to room temperature；Then timeliness 16 for the first time at 70~90 DEG C ~24 hours, then timeliness 6~24 hours at 140~260 DEG C, were air-cooled to room temperature；Aging temp selection is lower, when reaching peak Longer the time required to effect, alloy comprehensive mechanical property is higher, conversely, aging temp is higher, the time used in arrival peak timeliness is got over Short, alloy comprehensive mechanical property is relatively low.But two-stage time effect comprehensive mechanical property is more superior compared to single-stage aging, therefore more Suitable for disregarding the defense industry and field of aerospace of cost.
Performance test
One, mechanics properties testing
According to the standard of national standard GB228-2002, the fixed embodiment of every group of formulated component is limited in above-mentioned preparation process In the range of, then distinguished during the preparation process according to different extruding conditions and Ageing conditions, it is prepared as identical component and matches Than different group's materials of lower different preparation conditions, then by obtained each group Mg-Zn-Sn-Mn-Al deformed magnesium alloy material line It is cut into standard tensile specimen and carries out tension test, draw direction is parallel to the direction of extrusion.Gained stretches sample mechanical property As shown in table 2.
Table 2 is that each component mass percent determines in embodiment, according still further to different extruding conditions and Ageing conditions Difference Mg-Zn-Sn-Mn-Al series deformation magnesium alloy material obtained, tests the mechanical property of acquisition.
As shown in Table 2, the Mg-5.92Zn-4.23Sn-0.89Mn-0.58Al wrought magnesium alloy prepared in embodiment 5 is comprehensive Mechanical property is best.On the one hand, compared with the magnesium alloys such as conventional commercial wrought magnesium alloy AZ series and M1A series, As-extruded room Warm mechanical property increases substantially, and tensile strength is up to 422Mpa, and yield strength is up to 372Mpa, and room temperature comprehensive mechanical property is very To surmounting many rare-earth-contained magnesium alloys.On the other hand, this alloy high-temp intensity not only can be with part rare-earth-contained magnesium alloy intensity It compares favourably, and this alloy elongation percentage can achieve 70% or more, is the 2 times or more of other alloy elongation percentages.
Table 3 is the ambient temperature mechanical properties of typical magnesium alloy:
Table 4 is 150 DEG C of mechanical properties of typical magnesium alloy.
Two, microscopic examination
Fig. 3 is the X ray diffracting spectrum of the As-extruded Mg-Zn-Sn-Mn-Al series deformation magnesium alloy material of embodiment 5, by For Fig. 3 it is found that as Al content≤0.6wt.%, the second phase of alloy is mainly α-Mg, Mg32(Al,Zn)49、Mg2Sn、MnSn2With Al8Mn5, and as Al content increases, second phase volume fraction increases, and alloy mechanical property further gets a promotion；As Al > When 0.6wt%, alloy the second phase portions turn is AlMg2Zn、Mg2Sn、Mn2Sn and Al3Mn.The transformation of second phase is to alloy force It learns performance and produces tremendous influence, the mainly overall distribution of the second phase and the physical property of tracing it to its cause change.Phase The mass fraction of Zn is changed, mechanical property is more sensitive to the change of Al mass fraction, is primarily due to when Zn/Al mass When than < 10, alloy generates the low temperature bulk ternary phase AlMg being distributed along crystal boundary2Zn.The followed by variation of Al-Mn phase, Al3Mn phase For Al8Mn5, Al3Mn level off to crystal boundary nearby generate and size it is larger, be difficult to be dissolved after heat treatment, it is easy to form larger Stress raiser so that crack.It is finally MnSn2Transformation, since the content of Al is further up, further reduced Mn2The nucleation barrier of Sn, this second phase is easy and other high-temperature-phases such as Mg2Sn is generated together, destroys the crystalline substance of script high-temperature-phase Body structure, so that Mg2The strengthening effect that Sn can be played reduces.Therefore, because the transformation of the second phase, as Al >=0.6wt.% When, alloy mechanical property starts dramatic decrease.In conclusion alloy structure and mechanical property are very sensitive to Al content, pass through Many experiments example is finally determined various elements ingredient optimum quality ratio.
After the ternary phase diagrams such as Mg-Zn-Al, Mg-Al-Mn, obtained at optimal heat by a large amount of heat treatment experiments Science and engineering skill.Fig. 4 and Fig. 5 is the solid solution metallographic microscope and SEM of embodiment, and as seen from the figure, the second phase of alloy after heat treatment is substantially solid While dissolving into matrix, the phenomenon that not occurring burning, grain size can maintain 15 μm, this is mentioned for subsequent ageing strengthening Good basis is supplied.
Fig. 2 and Fig. 3 is fracture of the As-extruded Mg-Zn-Sn-Mn-Al wrought magnesium alloy of embodiment when stretching for 150 DEG C Sem analysis, by Fig. 2 with Fig. 3 it is found that the second of alloy mutually distribution and size it is highly uniform, and substantially dimple structure, thus The main faults mode that may determine that alloy is to be plastic deformation to leading pore type fracture.
Fig. 6 is dsc analysis, and as seen from the figure, as Al content increases, melting peak temperature is reduced, and illustrates alloy casting character It is improved.
Fig. 7 be Mg-Zn-Sn-Mn-Al series deformation magnesium alloy single-stage aging at different temperatures prepared by embodiment 5 and The age hardening curves of two-stage time effect, it is as seen from the figure, shorter to reach to peak value timeliness required time with the increase of aging temp, Hardness is lower, longer to reach to peak value timeliness required time with the reduction of aging temp, but hardness is higher.Therefore, military industry field Disregarding any art with space flight and aviation etc. can be using longer aging time come optimized alloy, to reach the best mechanics of alloy Performance.
Fig. 8 is the single-stage aging and two-stage time effect of the Mg-Zn-Sn-Mn-Al series deformation magnesium alloy prepared in embodiment 4~6 Age hardening curves, as seen from the figure, hardness obtained by two-stage time effect process is generally higher than single-stage aging, and therefore, civil field can With the single-stage aging using the short period come optimized alloy, to reach best cost performance.
Fig. 9 is the As-extruded longitudinal section microstructure of Mg-Zn-Sn-Mn-Al series deformation magnesium alloy prepared by embodiment 5 SEM, as shown, homogeneous grain size and tiny, size maintains 5 μm, and coarse white bright extruding streamline is high-temperature stable phase Mg2Sn, remaining nanoscale hardening constituent Dispersed precipitate is in crystal boundary and transgranular, in drawing by high temperature, high-temperature stable phase Mg2Sn and other Tiny high-temperature stable phase pinning crystal boundary hinders dislocation movement by slip, to guarantee the high temperature comprehensive mechanical property of alloy.
The high-intensity thermal deformation resistant magnesium alloy mean intensity of room temperature high-strength high-temperature high-ductility in the present invention containing aluminium is higher than normal The mechanical property of the As-extruded AZ system seen, M1A system and ZK system, expands the application range of magnesium alloy.And the requirement of equipment It is not high, and production cost is low, lays a solid foundation for later production application.Such as it is closed compared to traditional commerce magnesium Gold, such as ZK60 series magnesium alloy, cost has both good mechanical property while reduction.Compared to traditional AZ series magnesium alloy, Such alloy yield strength is low, and yield ratio is 0.33~0.43, and Shrinkage Porosity is serious, and mechanical behavior under high temperature is poor, uses temperature 120 DEG C are usually no more than, but this alloy at normal temperature and high temperature yield are than generally more than 0.7, significantly Optimum Synthesis mechanical property.This master If because for the main hardening constituent Mg of AZ series17Al12For, (150 DEG C or more) deformations at relatively high temperatures, Mg17Al12 It is mutually easy to be broken, but as deformation temperature declines, Mg17Al12Phase hardness increases, and deformation is easy in the phase surrounding matrix Middle generation micro-crack, this can adversely affect alloy mechanical property.For this alloy, original Mg-Al hardening constituent It is changed into Mg32(Al,Zn)49, the fusing point of the phase is higher than Mg17Al12Phase, and its strengthening effect is also significantly better than Mg17Al12Phase, Therefore comprehensive mechanical property is obviously improved.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be Various changes are made to it in form and in details, without departing from claims of the present invention limited range.

Claims (10)

1. a kind of high-intensity thermal deformation resistant magnesium alloy material, which is characterized in that its component includes: 5~7.15wt.%Zn, 4.1~ 6wt.%Sn, 0.6~2.2wt.%Mn, 0.2~0.8wt.%Al, inevitable impurity≤0.15%, surplus Mg.
2. high-intensity thermal deformation resistant magnesium alloy material according to claim 1, it is characterised in that: by mass percentage, institute It is composed of the following components to state magnesium alloy: Zn:5~6wt.%, Sn:4.1~5wt.%, Mn:0.6~1.5wt.%, Al:0.5~ 0.8wt.%, inevitable impurity≤0.15%, surplus are magnesium.
3. high-intensity thermal deformation resistant magnesium alloy material according to claim 2, it is characterised in that: the group of magnesium alloys is divided into: Zn:5.9wt.%, Sn:4.1wt.%, Mn:0.9wt.%, Al:0.6wt.%, inevitable impurity≤0.15%, surplus are Magnesium.
4. the preparation method of high-intensity thermal deformation resistant magnesium alloy material as described in claims 1 or 2 or 3, it is characterised in that: including with Lower step:
(1) melting: with pure Mg, pure Zn, pure Sn, pure Al, Mg-10wt.%Mn are raw material, by the quality hundred of the magnesium alloy component Divide ratio to carry out calculating ingredient, 150 ± 5 DEG C of pure magnesium ingot will be preheating to and be added in resistance furnace, heat to 720 ± 5 DEG C to institute It states pure magnesium ingot to melt to obtain Serum Magnesium, successively remaining alloy raw material is added after 720 ± 5 DEG C for Serum Magnesium temperature control The Serum Magnesium to abundant fusing, addition refining agent refining slag hitting stirring is warming up to 740 DEG C of ± 5 DEG C of 35~45min of heat preservation, then Slag hitting is stirred after secondary standing, keeps the temperature 10~20min, finally uses die cast, and magnesium alloy ingot is made；Entire fusion process In CO2And SF6Mixed gas protected lower progress；
(2) it machines: the oxide skin on magnesium alloy ingot surface in removal step (1)；
(3) Homogenization Treatments: Homogenization Treatments will be carried out through step (2) treated magnesium alloy ingot；
(4) hot extrusion: by the ingot casting of step (3) processing in 330 DEG C~360 DEG C 30~60min of preheating, then carrying out hot extrusion, A kind of strong mechanical performance wrought magnesium alloy of room temperature high-strength high-temperature high-ductility is made.
5. the preparation method of high-intensity thermal deformation resistant magnesium alloy material according to claim 4, it is characterised in that: extruded bars Heat treatment process are as follows:
1) solution treatment+single-stage aging processing:
I.e. first 400~440 DEG C solution treatment 1~6 hour, water quenching to room temperature；Then timeliness 6~24 is small at 140~260 DEG C When, it is air-cooled to room temperature.
6. the preparation method of high-intensity thermal deformation resistant magnesium alloy material according to claim 4, it is characterised in that: extruded bars Heat treatment process are as follows:
2) solution treatment+two-stage time effect processing:
I.e. first 400~440 DEG C solution treatment 1~6 hour, water quenching to room temperature；Then at 70~90 DEG C for the first time timeliness 16~ 24 hours, then timeliness 6~24 hours at 140~260 DEG C, were air-cooled to room temperature.
7. the preparation method of high-intensity thermal deformation resistant magnesium alloy material according to claim 4, it is characterised in that: step (1) In, the die cast is to be poured into Serum Magnesium in the cast iron casting mould for being preheating to 600 ± 5 DEG C.
8. the preparation method of high-intensity thermal deformation resistant magnesium alloy material according to claim 4, it is characterised in that: step (1) In, the CO2And SF6Mixed gas in SF6Shared volume fraction is 0.01%.
9. the preparation method of high-intensity thermal deformation resistant magnesium alloy material according to claim 4, it is characterised in that: step (3) In, the Homogenization Treatments specifically: the ingot casting after peeling is warming up to 310 DEG C~340 DEG C, keeps the temperature 14~16 hours, then It is warming up to 360 DEG C~380 DEG C again, keeps the temperature 2~3 hours, is finally warming up to 400 DEG C~420 DEG C, keeps the temperature 2~3 hours, it is air-cooled To room temperature.
10. the preparation method of high-intensity thermal deformation resistant magnesium alloy material according to claim 4, it is characterised in that: step (4) In, the hot extrusion specifically: in extrusion ratio be 25:1, extrusion speed 1~3mm/s, carry out heat under the conditions of 330 DEG C~360 DEG C It squeezes.
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JP2008069418A (en) * 2006-09-14 2008-03-27 Kumamoto Univ High strength magnesium alloy with excellent corrosion resistance
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CN106521278A (en) * 2016-12-29 2017-03-22 湘潭大学 High-strength magnesium-zinc-manganese-yttrium-cerium magnesium alloy and preparation method thereof
CN108385007A (en) * 2018-02-09 2018-08-10 湘潭大学 A kind of high performance heat resistant deformed magnesium alloy material of low cost and preparation method thereof

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JP2008069418A (en) * 2006-09-14 2008-03-27 Kumamoto Univ High strength magnesium alloy with excellent corrosion resistance
CN102230118A (en) * 2011-07-05 2011-11-02 重庆大学 Magnesium alloy of high intensity and high yield ratio and preparation method thereof
CN103695741A (en) * 2013-12-16 2014-04-02 中国科学院金属研究所 Mg-Zn-Al-Sn-Mn series magnesium alloy and preparation method thereof
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