CN105886804B - A kind of preparation method of high-performance Mg-Zn based alloy - Google Patents
A kind of preparation method of high-performance Mg-Zn based alloy Download PDFInfo
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- CN105886804B CN105886804B CN201610317857.5A CN201610317857A CN105886804B CN 105886804 B CN105886804 B CN 105886804B CN 201610317857 A CN201610317857 A CN 201610317857A CN 105886804 B CN105886804 B CN 105886804B
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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
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- 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
Abstract
A kind of preparation method of high-performance Mg-Zn based alloy, belong to technical field of metal material, after magnesium and zinc fusing, refining, it is cast into alloy cast ingot, and Equal-channel Angular Pressing processing is carried out to the alloy cast ingot after homogenization heat treatment, magnesium-zinc alloy is obtained, magnesium-zinc alloy is finally subjected to solution heat treatment.The present invention can make graininess laves MgZn of the interphase of magnesium-zinc alloy with equally distributed diameter at 100 nanometers to 200 nanometers2Based on phase, matrix grain size is below 10 microns, so that its mechanical property is significantly improved.
Description
Technical field
The invention belongs to the technology of preparing of technical field of metal material, more particularly to magnesium-zinc alloy.
Background technology
Mg-Zn based alloy is a kind of magnesium alloy with higher-strength, and in the cast condition, the centre of magnesium-zinc alloy is communicated
It is often block eutectic, with the rise of Zn content, the interphase content in material is increased.When the Zn-ef ficiency in magnesium-zinc alloy
When content exceedes mass percent 3%, even if fully after solution treatment, interphase is still suffered from magnesium-zinc alloy can not be complete
Dissolve and save.In the magnesium-zinc alloy of as-cast condition, main interphase is block Mg7Zn3Phase（That is Mg51Zn20Phase）
With a small amount of MgZn phases, the fusing points of both phases is respectively 341 DEG C and 325 DEG C, exceed in deformation or close to this temperature just
Magnesium alloy cracking is likely to cause, and magnesium alloy is a kind of difficult-to-machine material, the temperature of plastic deformation is usual more than 200 DEG C,
Temperature rise may also reach or close to this temperature in the case of drastic deformation, therefore the plastic working of magnesium-zinc alloy
Temperature range is very narrow, and difficulty of processing is larger.The plasticity of the more magnesium-zinc alloys of thick interphase is lower, so as to cause magnesium-zinc alloy
Crystallized ability declines at high temperature, and mechanical property at room temperature is relatively low.
Common interphase is except Mg in magnesium zinc bianry alloy7Zn3Mutually and outside MgZn phases there are Laves MgZn2Xiang He
Mg4Zn7It is equal, the wherein MgZn of Laves structures2Mutually compared with other interphases with higher heat endurance（Fusing point about 590
℃）With good mechanical property, and its crystal structure and magnesium are all hexagonal structure, and with matrix into half symbiosis and epibiosis, it is to carrying
High intensity has remarkable effect.
Severe plastic deformation（severe plasticity deformation, SPD）It is crystal grain thinning, reduces interphase
Size, reduce material anisotropic effective ways.Severe plastic deformation method includes Equal-channel Angular Pressing（equal-
channel angular pressing, ECAP）, reciprocating extrusion（cyclic-extrusion compression, CEC）、
Three-dimensional forging (multi-directional forging, MDF）Deng.Conventional research finds that ECAP can induce magnesium-zinc alloy
In a large amount of separate out ellipsoids or spherical Laves MgZn2Phase, this is for improving the shaping under material mechanical performance and high temperature
Performance is helpful.And do not had then under the processing conditions such as traditional extruding, rolling or only a small amount of Laves MgZn2Phase
Separate out.
The content of the invention
The present invention seeks to propose the preparation method of high-performance magnesium-zinc alloy inexpensive in one.
The present invention comprises the following steps：
1）After magnesium and zinc fusing, by stirring, refining treatment, zinc member in alloy cast ingot, the alloy cast ingot is cast into
Element accounts for the 4.0~12.0% of alloy gross mass；
2）Alloy cast ingot is subjected to homogenization heat treatment；
3）Equal-channel Angular Pressing processing is carried out to the alloy cast ingot after homogenization heat treatment, magnesium-zinc alloy is obtained；
4）Magnesium-zinc alloy is subjected to solution heat treatment.
The technology of the present invention principle：Deng channel pressings（ECAP）The crystal grain of magnesium-zinc alloy can be refined, makes eutectic phase broken simultaneously
Distribution uniformity, and greatly improve laves MgZn2The speed mutually separated out, the laves MgZn of precipitation2It is mutually main spherical in shape or ellipse
Spherical, this can not be obtained by the common plastic working technique such as extruding, forging, rolling.Carried out after ECAP at solid solution
Reason can make the Mg separated out under as cast condition7Zn3Eutectic phase decomposition, and laves MgZn2Mutually with higher heat endurance, therefore
It can be retained after heat treatment.Member in magnesium-zinc alloy can be made by repeating the process of severe plastic deformation and solution treatment
The distribution of element is more uniform, eliminates the eutectic phase of big bulk, the substitute is tiny equally distributed graininess phase, and
And interphase is largely converted into the laves MgZn with more preferably reinforcing effect2Phase.At multi-pass severe plastic deformation
The material of reason refines abundant crystal grain, and crystallite dimension can be reduced to micron order even submicron order.In second-phase strength and fine grain
In the presence of strengthening mechanism, the mechanical property of magnesium-zinc alloy is also significantly improved.
Interphase by Equal-channel Angular Pressing crystal grain thinning and is converted to laves MgZn by the present invention2Phase.
Method of the present invention by carrying out severe plastic deformation and solution heat treatment simultaneously to magnesium-zinc alloy, reduction magnesium zinc is closed
The size of block eutectic in gold, while controlling species, size and the pattern of precipitated phase, reaches the room temperature mechanics for improving magnesium-zinc alloy
The purpose of performance and hot forming performance.
The advantage of the invention is that handling magnesium-zinc alloy by severe plastic deformation method induces laves MgZn2Xiang Xi
Go out, and other interphases are dissolved into matrix by appropriate solid solution treatment process, repeat severe plastic deformation and solid
The technique of molten processing can control size, distribution and the species of crystallite dimension and interphase.The technology can make magnesium-zinc alloy
Graininess laves MgZn of the interphase with equally distributed diameter at 100 nanometers to 200 nanometers2Based on phase, matrix grain
Size is below 10 microns, so that its mechanical property is significantly improved.
Further, the present invention is in the step 1）In, it is additionally added in stirring in calcium, tin, manganese, aluminium or rare earth element
It is at least one.Calcium：Calcium mainly forms Mg as alloying element with magnesium2Ca phases, play a part of improving intensity；Tin is used as alloy member
Element can play solution strengthening effect, and tin also can be with magnesium formation Mg2Sn phases, improve alloy strength；Aluminium has certain consolidate in magnesium
Solubility can play a part of solution strengthening, and aluminium can form Mg with magnesium17Al12Phase, can also be with magnesium and zinc formation ternary eutectic
Compound, plays a part of improving alloy strength；Manganese mainly combines to form ternary compound as alloying element with aluminium, iron,
Reduce the adverse effect of iron in the magnesium alloy；Rare earth element can effectively remove oxide during magnesium alloy smelting, reduction
The harm of field trash.Rare earth element can play a part of solution strengthening with magnesium formation solid solution.Rare earth element can with magnesium with
And other elements formation multiple compounds, so as to improve alloy strength.
Temperature≤325 DEG C of the homogenization heat treatment.Component segregation can effectively be eliminated.In the casting solidification process of alloy
In, thick eutectic structure is easily formed on matrix crystal boundary, thick eutectic is easily sent out in the plastic history of material
Raw cracking, causes material processing characteristics to decline.Homogenization Treatments can be such that the solute atoms in eutectic is migrated by spreading,
It is eutectic size reduction.Phase constituent is Mg51Zn20 phases (i.e. Mg7Zn3 phases) and MgZn phases in the middle of in as cast condition magnesium-zinc alloy, and it melts
Point is respectively 341 DEG C and 325 DEG C, is heat-treated more than this temperature, and MgZn, which meets, to be melted and hole is formed in cooling procedure, no
Beneficial to follow-up plastic working, therefore magnesium-zinc alloy Homogenization Treatments temperature requirement is below 325 DEG C.
The Equal-channel Angular Pressing is processed as multi-pass, and the deformation temperature of each passage is 200 ± 50 DEG C.
It is a kind of severe plastic deformation technology Deng channel pressings, sample can be improved by the multi-pass processing to sample
Dependent variable, thus refining grain size, and make the second distributed mutually of material uniform, but the continuous inferior channel pressings of multiple tracks can be led
Material processing hardening is caused, is easily ftractureed, therefore for magnesium-zinc alloy, the continuous number of times for waiting channel pressings is no more than 6 passages.
The deformation temperature of magnesium-zinc alloy is typically not less than 150 DEG C, and magnesium-zinc alloy easily ftractures at less than 150 DEG C, with carrying for temperature
The processing characteristics of high magnesium-zinc alloy is significantly improved, but waits channel pressings not good to the thinning effect of crystal grain at high temperature, and is worked as
When temperature is more than 300 DEG C, the interphase of magnesium-zinc alloy, the intensity of such as Mg51Zn20 phases and MgZn phases is remarkably decreased, so as to cause
Material is ftractureed in deformation process, therefore processing temperature should be selected in alap temperature range.
Temperature≤325 DEG C of the solution heat treatment, the time is 1~2 hour.Solid solubility temperature 325 DEG C the following is in order to
Avoid Mg51Zn20Mutually melted with MgZn phases and form hole, the time was in order to by metastable Mg at 1 ~ 2 hour51Zn20Xiang He
MgZn phased solns, and avoid matrix crystal grain grow up it is too fast.
To step 3）With 4）Carry out circulate operation at least twice.Make to analyse in magnesium-zinc alloy supersaturated solid solution Deng channel pressings
Go out Laves MgZn2Phase, refines matrix grain.And solution heat treatment comprehends the Mg caused in magnesium-zinc alloy51Zn20Mutually mixed with MgZn
Solution, crystal grain has been grown up, and eliminates processing hardening.The purpose for carrying out circulate operation more than twice is, by Mg51Zn20Phase and MgZn
Mutually fully dissolve and be converted into the more stable Laves MgZn of thermodynamics2Phase, is formed with Laves MgZn2Mutually to be main middle
The magnesium-zinc alloy microscopic structure of phase, so as to improve magnesium-zinc alloy performance.
Brief description of the drawings
Fig. 1 is Mg-6Zn（Zinc percentage by weight 6%）Alloy passes through different Equal-channel Angular Pressing and equal channel angular
Extruding and the mechanical property figure after the processing of solution heat treatment group technology.
Embodiment
First, preparation technology：
1st, first magnesium and zinc are melted, then adds other elements, alloy cast ingot is cast into by stirring, refining treatment etc..
The chemical composition mass percent of the alloy is：Zinc 4.0~12.0%, remaining is magnesium and inevitable impurity, together
When the alloy in can also add the one or several kinds in calcium, tin, manganese, aluminium and rare earth element.
Following table is the raw material proportioning table of each example（Unit is：kg）
2nd, each alloy cast ingot carries out less than 325 DEG C of Homogenization Treatments respectively by more than, eliminates component segregation.
3rd, each ingot casting after Homogenization Treatments is subjected to Equal-channel Angular Pressing（equal-channel angular
pressing, ECAP）, multi-pass processing can be carried out, the deformation temperature of each passage is at 200 ± 50 DEG C.
4th, magnesium-zinc alloy after severe plastic deformation is handled carries out solution heat treatment, heat treatment temperature below 325 DEG C,
Material within 2 hours, is then carried out Equal-channel Angular Pressing by the time again.
The operation of the above the 3rd, 4 can be carried out with circulating repetition.
2nd, interpretation of result：
With Mg-6Zn（Zinc percentage by weight 6%）Exemplified by alloy, the Mg-6Zn alloys of as cast condition are designated as No. 1；By 200
DEG C passage of Equal-channel Angular Pressing 2 is designated as No. 2；By being designated as No. 3 in 200 DEG C of passages of Equal-channel Angular Pressing 6；By two
The secondary passage of Equal-channel Angular Pressing 2（200 DEG C of passages of Equal-channel Angular Pressing 2, then in 320 DEG C of Homogenization Treatments 1 hour,
200 DEG C of passages of Equal-channel Angular Pressing 2 are carried out again）It is designated as No. 4；By three passages of Equal-channel Angular Pressing 2（200 DEG C etc.
The passage of channel angular extrusion 2, then in 320 DEG C of Homogenization Treatments 1 hour, 200 DEG C of passages of Equal-channel Angular Pressing 2 finally exist
320 DEG C of Homogenization Treatments 2 hours, then carry out 200 DEG C of passages of Equal-channel Angular Pressing 2）It is designated as No. 5.No. 4 and No. 5 employ this
The method of technology.
Fig. 1 is Mg-6Zn（Zinc percentage by weight 6%）Alloy passes through different Equal-channel Angular Pressing and equal channel angular
Extruding and the mechanical property figure after the processing of solution heat treatment group technology.
YS represents room-temperature yield strength in figure, and UTS represents room temperature tensile strength, and El. represents room temperature fracture elongation；as-
Casted represents as-cast specimen, and 200-2p represents examination of the cast alloy after 2 passage Equal-channel Angular Pressings processing at 200 DEG C
Sample, 200-6p represents sample of the cast alloy after 6 passage Equal-channel Angular Pressings processing at 200 DEG C, and 2*200-2p represents 2
The sample of 2 passage Equal-channel Angular Pressings at secondary 200 DEG C, and once 320 between continuous 2 200 DEG C of Equal-channel Angular Pressings
The solution heat treatment of 1 hour at DEG C, 3*200-2p represents the sample of 32 passage Equal-channel Angular Pressings at 200 DEG C, per continuous 2
The once solution heat treatment of 1 hour at 320 DEG C between secondary 200 DEG C of Equal-channel Angular Pressings.
As seen from Figure 1：After 200 DEG C of 2 inferior channel pressings in road, alloy strength has obvious rising, and proceeds to 6
Yield strength and tensile strength do not rise not only after passage extruding, are declined slightly on the contrary, this is due to MgZn2Mutually long roughening
Cause.And the sample 4 of the passage of Equal-channel Angular Pressing 2 twice is used, the intensity of No. 2 and No. 3 samples of strength ratio is carried
Height, elongation percentage is declined slightly, and the intensity that sample 5 then continues to rise.This explanation is for magnesium-zinc alloy, and this technology can be in refinement
MgZn in magnesium-zinc alloy is given full play on the basis of crystal grain2The effect of phase precipitation strength, and traditional continuous equal channel angular are squeezed
Pressure, which is compared, can preferably improve the intensity of magnesium-zinc alloy.
Claims (4)
1. a kind of preparation method of high-performance magnesium-zinc alloy, comprises the following steps：
1）After magnesium and zinc fusing, by stirring, refining treatment, it is cast into Zn-ef ficiency in alloy cast ingot, the alloy cast ingot and accounts for
The 4.0~12.0% of alloy gross mass；
2）Alloy cast ingot is subjected to homogenization heat treatment；
3）Equal-channel Angular Pressing processing is carried out to the alloy cast ingot after homogenization heat treatment, magnesium-zinc alloy is obtained；
4）Magnesium-zinc alloy is subjected to solution heat treatment；
It is characterized in that to step 3）With 4）Carry out circulate operation at least twice；Temperature≤325 DEG C of the solution heat treatment, when
Between be 1.5 hours~2 hours.
2. the preparation method of high-performance magnesium-zinc alloy according to claim 1, it is characterised in that in the step 1）In, stirring
Calcium, tin, manganese, at least one of aluminium or rare earth element are additionally added when mixing.
3. the preparation method of high-performance magnesium-zinc alloy according to claim 1, it is characterised in that the homogenization heat treatment
Temperature≤325 DEG C.
4. the preparation method of high-performance magnesium-zinc alloy according to claim 1, it is characterised in that the Equal-channel Angular Pressing
Multi-pass is processed as, the deformation temperature of each passage is 200 ± 50 DEG C.
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| CN102304653A (en) * | 2011-09-09 | 2012-01-04 | 华南理工大学 | High-plasticity two-phase yttrium-containing magnesium-lithium-aluminum alloy and preparation method thereof |
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