CN109943759A - High-toughness heat-resistant Mg-Er alloy and preparation method thereof suitable for gravitational casting - Google Patents
High-toughness heat-resistant Mg-Er alloy and preparation method thereof suitable for gravitational casting Download PDFInfo
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Abstract
The present invention provides the high-toughness heat-resistant Mg-Er alloys and preparation method thereof for being suitable for gravitational casting, the alloy composition mass percentage content are as follows: 4.0~10.0%Er, 2.0~6.0%Zn, 0.5~1.2%Al, 0.1~0.3%Mn, 0.01~0.08%M, surplus Mg；Wherein M is Ti, one or two kinds of elements in B.Preparation method: (1) by Mg-Er alloying component ingredient is carried out；(2) technical pure magnesium ingot is melted；(3) 700 DEG C are warming up to, industrial-purity zinc and Mg-Er and Mg-Mn intermediate alloy are melted；(4) 730 DEG C are warming up to, after technical pure aluminium ingot, Al-Ti, Al-Ti-B, Al-B intermediate alloy whole fusing is added, refining obtains magnesium alloy fused mass；(5) gravitational casting；(6) second level solid solution, artificial aging processing.For alloy of the invention after the heat treatment of gravitational casting, second level solution treatment and artificial aging, room temperature tensile intensity is 296MPa, elongation percentage 18%；Drawing by high temperature tensile strength is 215MPa at 200 DEG C, and elongation percentage 23% meets the industries such as aerospace, automobile, telecommunication to light-weighted high demand.
Description
Technical field
The present invention relates to the high-toughness heat-resistant Mg-Er alloys for being suitable for gravitational casting, meet aerospace, automobile, telecommunication etc.
The high demand that industry develops lightweight.The invention further relates to the high-toughness heat-resistant Mg-Er alloy preparations for being suitable for gravitational casting
Method belongs to industrial magnesium alloy and manufacturing field.
Background technique
For magnesium alloy as most light engineering metal material (density of magnesium is 2/3, the 1/4 of steel of aluminium), specific strength is obvious
Higher than aluminium alloy and steel, although specific stiffness is suitable with aluminium alloy and steel, it is much higher than engineering plastics, while there is good casting
Property, the series of advantages such as machinability is good, thermal conductivity is good, damping and amortization and electromagnetic shielding capability are strong and are easily recycled, navigating
The fields such as sky, space flight, automobile, electronics and defence and military have a wide range of applications.Magnesium alloy becomes substitution aluminium alloy, steel
With engineering plastics to realize light-weighted ideal material, wherein it is aluminium alloy that it is maximum, which to substitute potentiality,.Cast aluminium alloy gold has must
The toughness and tenacity and thermal stability wanted are widely used for production engine cylinder body and the parts such as cylinder cap and wheel hub at present, represent
Alloy be A354, A356 and A380.If magnesium alloy replaces cast aluminium alloy gold, it must have equivalent toughness and tenacity, and
It is inexpensive, be easy to cast.Gravitational casting refers to that molten metal injects the casting method of casting mold under terrestrial gravitation effect, including sand mold pours
Casting, model casting, permanent mold casting etc..Compared with the alloy die cast technique generallyd use at present, the investment of gravitational casting at
Originally it is greatly lowered, is the main method for producing complex geometry casting.
Earliest, the Atomic radiuses difference of main alloy element aluminium and magnesium is larger while in magnesium for the application of Mg-Al class magnesium alloy
In have biggish solid solubility, play solution strengthening and precipitation strength in the alloy.Find that a small amount of Mn is significant in nineteen twenty-five
After the corrosion resistance for improving Mg-Al-Zn system magnesium alloy, AZ (such as AZ91) and AM system magnesium alloy (such as AM60, AM50) develop into mesh
Preceding most widely used commercialization magnesium alloy.However the high temperature creep property of AZ and AM magnesium alloy is very poor, it is lower than Aluminium Alloys in Common Use
An order of magnitude is more, and the tensile strength when temperature is higher than 150 DEG C reduces rapidly, and reason is during high-temerature creep
Mg of the oversaturated α-Mg matrix in grain boundaries17Al12Mutually discontinuous precipitation.By the way that alloying element is added to improve precipitated phase
The heat resistance of characteristic (crystal structure, form and thermal stability) Lai Tigao Mg-Al alloy, but its room temperature and mechanical behavior under high temperature
It is still unable to reach the level of cast aluminium alloy gold, seriously limits its application development.For example, application publication number is CN109136701A
Patent document (a kind of sand mold gravitational casting magnesium alloy materials and preparation method thereof) disclosed in magnesium alloy component content are as follows: 3.5
~4.5wt.%Al, the mischmetal of one or more of La, Ce, Pr of 0.5~4.5wt.%, 0.2~0.5wt.%Mn,
One or more of Gd, Y, Sm, Nd, Er, Eu, Ho, Tm, Lu, Dy, Yb of 0.01~2.5wt.% mischmetal, remaining is
Mg；The best ambient temperature mechanical properties for the alloy reported: tensile strength 231MPa, elongation percentage 11.4%.
Maximum solid solution degree of the zinc Zn in Mg is up to 6.2wt%, is the important alloy element of high-strength magnesium alloy.Typically
Mg-Zn series cast magnesium alloy includes ZK51A and ZK60A, and deforming alloy includes ZK21A, ZK31, ZK40A, ZK60A and ZK61 etc..
Increase with Zn content, the tensile strength and yield strength of alloy improve, and elongation after fracture is declined slightly, but casting character, work
Skill plasticity and welding performance deteriorate, and especially because freezing range is wide, (such as the freezing range of ZK60 is up to 265 DEG C, Journal
Of Materials Science, 45 (14) (2010) 3797-3803), cause its hot cracking tendency extremely serious.Rare earth elements RE
(rare earth element) is all to the Grain Refinement Effect of magnesium alloy to the beneficial effect and zirconium of magnesium alloy strength performance
In nineteen thirties discovery, EK31 becomes in Mg-Zr class and opens earliest in Mg-RE-Zr system (EK30, EK31, EK41)
Send out high temperature cast magnesium alloy successful.Magnesium-rare earth alloy based on rare earth RE element has excellent aging hardening effect, a variety of
It is successively developed with the novel magnesium alloy that RE is main added elements, such as WE54, WE43 alloy of Mg-Y system.Application publication number
A kind of high strength heat resistant magnesium conjunction is disclosed for the patent document (high-strength heat-resisting magnesium alloy and preparation method thereof) of CN1676646A
The preparation method of gold, the component and its weight percent of the Mg-Gd-Y-Zr (- Ca) magnesium-rare earth invented are as follows: 6~15%
Gd, 1~6%Y, 0.35~0.8%Zr, 0~1.5%Ca, the total amount of impurity element S i, Fe, Cu and Ni are less than 0.02%, surplus
For Mg.However, crystallite dimension reaches 90 μm when carrying out sand casting using such alloy, cast T6 state alloy tensile strength,
Yield strength and elongation percentage are only 295MPa, 212MPa and 2.2% (the patent text that application publication number is CN104928548A respectively
Offer a kind of disclosed high-strength heat-resistant magnesium alloy and preparation method thereof suitable for sand casting)；Simultaneously although the addition of Ca improves
The yield strength and elevated temperature strength of alloy also increased dramatically the solidification temperature range of alloy, increase hot cracking tendency, reduce conjunction
The processing performance of gold.
The solid solubility of heavy rare earth element Er in the magnesium alloy is up to 32.7wt.%, significantly larger than other common rare earth elements,
There are strong solution strengthening and ageing strengthening effect.It is similar to Mg-Y alloy system, cheap Zn is added in Mg-Er alloy,
More obvious action not only is woven with to the Precipitation group for regulating and controlling the alloy system, but also can under the conditions of different Zn/Er ratios
To form a variety of hardening constituents: the icosahedral quasicrystal easy to form when mass ratio >=2.35 Zn/Er (atomic ratio >=6.0) in alloy
Body structure I phase (Mg3Zn6Er)；When Zn/Er mass ratio (atomic ratio is between 1.5 and 6.0) between 0.59 and 2.35 in alloy
When face-centred cubic structure W phase (Mg easy to form3Zn3Er2) and I phase；When in alloy Zn/Er mass ratio between 0.39 and 0.59 it
Between (atomic ratio is between 1.0 and 1.5) when W phase and long period stacking order structure LPSO phase (Mg easy to form12ZnEr)；Work as alloy
LPSO phase (Journal of Alloys and easy to form when middle mass ratio≤0.39 Zn/Er (atomic ratio≤1.0)
Compounds,602(2014)32-39；Acta Materialia,68(0)(2014)325-338).A variety of Mg-Er-Zn strengthen
The room temperature intensity and high-temperature behavior that mutually can be further improved magnesium alloy, in addition to hardening constituent W, the elasticity modulus of LPSO phase and micro-
Hardness is more much higher than pure magnesium, can significantly improve the intensity and plasticity of magnesium alloy, alloy is made to show excellent synthesis
Mechanical property.The study found that only when rare earth element is that Y, Gd, Er, Dy, Ho, Tb, Tm can form LPSO knot in Mg-RE-Zn system
Structure (Materials Transactions, 48 (11) (2007) 2986-2992).Application publication number is the special of CN104894447A
The composition of alloy disclosed in sharp document (a kind of magnesium-rare earth and its preparation process of stratiform/needle-shaped two-phase composite strengthening) and its
Mass percent is respectively as follows: 6~25%Er, 4~10%Zn, surplus Mg, wherein the quality additional proportion of Er/Zn be 1.5~
3.Preparation method are as follows: Mg-Er intermediate alloy is placed in crucible, is heated up under protective atmosphere；When furnace temperature rises to 750
After~820 DEG C of temperature ranges, intermediate alloy fusing, after keeping the temperature 10~20min, stirring slagging-off；Then, smelting temperature is reduced extremely
740~800 DEG C, magnesium ingot is added, after keeping the temperature 10~20min, stirring slagging-off；Continue to reduce temperature to 700~780 DEG C, add Zn,
It stirs and removes the gred；Continue to increase temperature, after temperature is risen to 760~800 DEG C, stirs aluminium alloy, slagging-off；Finally, by aluminium alloy
It keeps the temperature, stand more than half an hour at such a temperature, be cooled to 720~60 DEG C to aluminium alloy and be cast in mold, alloy is solidifying
Lamellar phase is generated in the process；The alloy prepared is placed in heat-treatment furnace in 450~525 DEG C of progress solution treatment, heat preservation
Between 5h~30h, the alloy after solution treatment has needlelike phase precipitation.The invention are as follows: because alloy is without thin
Change crystal grain element, crystallite dimension is up to 100 μm or more in Detailed description of the invention and it is necessary to pass through higher temperature solid solution organization of regulation control；
Rare earth element er content is too high to cause its density excessive, while expensive rare earth price causes the invention to be difficult industrially to carry out
Large-scale application.The patent document that application publication number is CN102212727A is (a kind of to improve the microcosmic of magnesium alloy temperature-room type plasticity
Microstructure refinement method) a kind of microstructure thinning method for improving magnesium alloy temperature-room type plasticity is disclosed, this method includes following step
It is rapid: (1) to be to clean the Mg-Zn-Er alloy surface obtained mixed containing I phase, W phase or I phase and W first, remove
Then oxide skin is split, be placed in the melting resistance furnace that temperature is 720~800 DEG C and kept the temperature, melted to alloy
Afterwards, heating power supply is closed, is stirred evenly, after standing 10~25min, furnace temperature is risen to 720~800 DEG C again, heat preservation 5~
10min closes heating power supply, and sets furnace temperature as 650~720 DEG C, after temperature is stabilized to 650~720 DEG C, by 0.01~
The Al of 1.0wt.% is added in aluminium alloy, stirring, and after 650~720 DEG C of heat preservations stand 10~25min, by alloy casting
In low-carbon steel mold；(2) step (1) the Mg-Zn-Er alloy solid solution obtained containing a small amount of Al element is handled, at solid solution
Managing temperature is 350~450 DEG C, and after keeping the temperature 2.5~15h, spherical or/and island mutually disappears in alloy, in matrix and grain boundaries shape
At a kind of acicular second phase, it is distributed more disperse.The invention are as follows: the invention is using Zn as host element
Mg-Zn-Er alloy in, Zn/Er mass forms the tissue containing icosahedral quasicrystal phase, freezing range is big, can only carry out than too high levels
Gravitational casting is not suitable for die casting.The Mg-Zn-Er alloy that the inventive method needs first to prepare phase containing I, W phase or I phase and W is mixed
Then ingot, and add Al after carrying out remelting carries out gravitational casting and carries out solid solution to homogenize and subsequent hot extrusion, complicated
Preparation process be difficult industrially to be applied on a large scale.Under the conditions of conventional coagulation, Mg-Er-Zn alloy grain is coarse,
Its precipitated phase is usually in coarse reticular structure, is degrading its mechanical property, it is necessary to by thermal deformation or heat treatment solid solution and
Timeliness adjusts precipitate size and strengthens phase separation to play it.
Mg-Er-Zn alloy is usually added into Zr as grain refining element, to refine its coarse microstructure.At present
Report adds Zr mode to have the halogen of sponge Zr, Zr, Zn-Zr and Mg-Zr intermediate alloy etc., and wherein Mg-Zr intermediate alloy has and makes
The advantages that with facilitating, being mingled with less with good in refining effect, be the major way for being currently fed Zr.Such as: application publication number is
Mg- disclosed in a kind of patent document (high-strength heat-resistant magnesium alloy and preparation method thereof suitable for sand casting) of CN104928548A
Contain the K of 0.2~0.6%Zr in the preparation method of Gd-Y-Ag-Zr (B) magnesium-rare earth by addition2ZrF6Salt-mixture
(K2ZrF6- NaCl-KCl) and B2O3, crystal grain during inhibiting alloy in sand casting and to be then dissolved grows up.Add at present
Zr crystal grain refinement still has many problems: firstly, the preparation process of Mg-Zr intermediate alloy is complicated, energy consumption is high, leading to its price
Valuableness, therefore product cost can be improved using Mg-Zr intermediate alloy refinement crystal grain；Secondly, Zr chemical activity is strong, hold at high temperature
Easy to react with atmosphere, furnace gas, when using steel crucibles, when melt temperature is higher than 750 DEG C, Zr is easy anti-with the Fe in crucible
It answers, generates stable intermetallic compound Fe2Zr, it is high that these result in Zr loss；Many Zr in Mg-Zr intermediate alloy be with
The form of large scale simple substance particle exists, and since the fusing point of Zr is high (1852 DEG C), Zr particle is difficult to dissolve in melt, in addition Zr
Density much larger than Serum Magnesium density (density of Zr be 6.52g/cm3, the density of pure Serum Magnesium is 1.58g/cm3), it is easy to heavy
It forms sediment to crucible bottom, causes the recovery rate of Zr low.
Summary of the invention
The present invention is unable to reach the casting aluminium such as A380 to solve existing cast magnesium alloy because of obdurability, heat resistance deficiency
The performance of alloy, the professional problem for causing its application to be extremely restricted, provides the high-toughness heat-resistant Mg- suitable for gravitational casting
Er alloy and preparation method thereof, for the alloy after gravitational casting is heat-treated, the room temperature tensile intensity of alloy is 296MPa, elongation percentage
18%；Drawing by high temperature tensile strength is 215MPa, elongation percentage 23% at 200 DEG C.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical solutions:
High-toughness heat-resistant Mg-Er alloy suitable for gravitational casting of the invention, the element including following mass percent:
4.0~10.0%Er, 2.0~6.0%Zn, 0.5~1.2%Al, 0.1~0.3%Mn, 0.01~0.08%M, surplus be Mg and
Other inevitable impurity, wherein one or both of M Ti, B.
The present invention is suitable for the high-toughness heat-resistant Mg-Er alloy innovative point of gravitational casting:
(1) in alloy design in addition to common metal Zn, Al, Mn and a small amount of Ti and B element, the present invention selects heavy rare earth
Element Er is as its alloy element.Alloy element Er and Zn and matrix Mg element form ternary Mg-Er-Zn hardening constituent, special
It is not in the range of Zn/Er mass ratio 0.2~0.7, on the one hand, alloy of the present invention primarily forms long period stacking order structure
LPSO(Mg12ZnEr) phase and face-centred cubic structure W (Mg3Zn3Er2) phase, it is high-melting-point phase；With binary Mg-Er hardening constituent ratio,
The high-temperature stable of ternary Mg-RE-Zn hardening constituent LPSO and W in magnesium matrix is more preferable, avoids causing due to precipitation strength phased soln
Reduced performance, effectively enhance the room-temperature mechanical property and high temperature of the high-toughness heat-resistant Mg-Er alloy suitable for gravitational casting
Performance, especially room-temperature yield strength double.On the other hand, the present invention overcomes traditional Mg-Zn-Er alloys because excessively high
Zn content cause freezing range excessive and be also easy to produce thermal fragmentation defect, alloy toughness and tenacity and Production Practice of Casting Technologies decline technology
Problem.
(2) Mg-Er-Zn alloy precipitated phase under the conditions of conventional coagulation is usually in coarse reticular structure, is degrading its power
Learn performance, it is often necessary to which precipitate size is adjusted to play the work of its hardening constituent by thermal deformation or heat treatment solid solution and timeliness
With.Such alloy is usually added into Zr as grain refining element, and Al, Mn and rare earth Er alloy are contained in alloying element of the invention
Element, these elements form Al in conjunction with Zr3The compounds such as Zr and being deposited to crucible bottom makes zirconium not play Grain Refinement Effect.Separately
On the one hand, studies have shown that the thermal structure stability of the Mg-Er-Zn alloy of addition Zr refinement is poor, the crystal grain in 550 DEG C of heat preservations
Sharply it is roughened, high-temperature behavior is caused to be greatly lowered.To solve the above-mentioned problems, 0.5-1.2% is added in alloy of the invention
Al substitutes Zr, forms the high-melting-point Al of disperse3Er phase has not only refined the tissue of alloy, but also has ensured with high-temperature-phases such as LPSO
The high-temperature stability of Magnesium Alloy.Al plays composite crystal grain fining together with a small amount of Ti and B simultaneously, further refines
Alloy structure, improves the obdurability of alloy.A small amount of Mn is added in alloying element of the invention, can not only promote LPSO
The formation of phase improves the high-temperature stability of alloy, and improves the corrosion resistance of magnesium alloy.
(3) in order to reduce the hot cracking tendency in Mg-Er-Zn alloy casting process, Zn/Er matter is limited in alloy of the invention
Amount is than 0.2~0.7 and (Zn+Al)/Er mass ratio is 0.3~0.8.Under this mass ratio, alloy of the invention obtain compared with
Narrow freezing range improves the casting technique of alloy to overcome the hot cracking tendency in Mg-Er-Zn alloy casting process
Performance.
The preparation method of the above-mentioned high-toughness heat-resistant Mg-Er alloy suitable for gravitational casting, includes the following steps:
(1) with due regard to after scaling loss, by above-mentioned Mg-Er alloying component and stoichiometric ratio, raw material (technical pure needed for calculating
Magnesium ingot, industrial-purity zinc, technical pure aluminium ingot, Mg-Er intermediate alloy, Mg-Mn intermediate alloy, Al-Ti intermediate alloy, in Al-Ti-B
Between alloy and Al-B intermediate alloy) dosage；It will be in technical pure magnesium ingot, industrial-purity zinc, technical pure aluminium ingot and Mg-Er and Mg-Mn
Between alloy go removing oxide layer and dry be preheated to 200 DEG C.
(2) after the technical pure magnesium ingot for accounting for crucible height 25% being fused into molten bath at 680 DEG C, it is passed through protective gas, is added
Enter remaining magnesium ingot.The protective gas is argon gas, or the SF for being 0.2% containing volume fraction6And CO2Mixed gas (i.e. SF6Body
Fraction is 0.2%, CO2Volume fraction be 99.8%).
(3) after magnesium ingot all fusing, 700 DEG C are warming up to, industrial-purity zinc and Mg-Er and Mg-Mn intermediate alloy point is more
(2~4) secondary addition, and keep temperature constant at 700 DEG C, it is stirred until all melting, and keep the temperature 30min.Preferably,
The Mg-Er intermediate alloy is MgEr25 or MgEr30, and the Mg-Mn intermediate alloy is MgMn10.
(4) 40~60min before gravitational casting is warming up to 730 DEG C, closes among technical pure aluminium ingot to be sequentially added, Al-Ti
Gold, Al-Ti-B intermediate alloy, Al-B intermediate alloy all after fusing, are added refining agent and are refined, furnace temperature is risen to 750 DEG C
Heat preservation stands 10~20min, and promotion is mingled with sedimentation, obtains magnesium alloy fused mass.The Al-Ti-B intermediate alloy is AlTi5B1, institute
Stating Al-B intermediate alloy is AlB3 or AlB8, and the Al-Ti intermediate alloy is AlTi5 or AlTi10.The quality of the refining agent
Percent composition are as follows: 55%KCl, 25%CaCl2, 5%CaF2, 15%BaCl2.The refining agent additive amount is raw material gross weight
1.0~3.5%, refining temperature when refining agent refining is added is 720~730 DEG C, the mixing time 10 of refining treatment~
15min。
(5) magnesium alloy fused mass is cooled between 720~740 DEG C and is removed the gred, poured into melt by gravitational casting
It is pre-heated in 25~150 DEG C of sand mold type molds or 180~250 DEG C of metal type dies, it is tough resistance to that the height is obtained after cooling
Mg-Er alloy is made in hot-cast.
(6) height needed for successively carrying out second level solution treatment, artificial aging processing acquisition to resulting cast alloy is tough
Heat-resistant cast Mg-Er alloy.
The second level solutionizing step of the high-toughness heat-resistant Mg-Er alloy suitable for gravitational casting: by cast alloy
It is put into solid solution furnace, is warming up to 200 DEG C with 5 DEG C/min, being passed through protective gas, (protective gas is argon gas, or containing volume point
The SF that number is 0.2%6And CO2Mixed gas (i.e. SF6Volume fraction is 0.2%, CO2Volume fraction be 99.8%)), after
It is continuous to be warming up to 480~490 DEG C of first order solid solubility temperature with 5 DEG C/min, keep the temperature 36~48h；Then it is warming up at a slow speed with 10 DEG C/h
535~545 DEG C of second level solid solution temperature, water hardening is carried out on fast transfer to quenching unit after keeping the temperature 1~2h.
The artificial aging of the high-toughness heat-resistant Mg-Er alloy suitable for gravitational casting is handled, at the artificial aging
The step of science and engineering skill are as follows: quenched alloy is put into aging furnace, artificial aging treatment temperature 185 is warming up to 5 DEG C/min
It~215 DEG C, comes out of the stove after keeping the temperature 12~36h and is air-cooled to room temperature.
The second level solid solution treatment process parameter are as follows: 480~490 DEG C of first order solid solubility temperature, soaking time 36~
48h；535~545 DEG C of second level solid solubility temperature, 1~2h of soaking time；
The artificial aging treatment process parameter: 185~215 DEG C of aging temp, 12~36h of soaking time.
The innovative point of the preparation method of high-toughness heat-resistant Mg-Er alloy provided by the invention suitable for gravitational casting: (1) exist
700 DEG C are added the Mg-Er intermediate alloy of easy scaling loss, and fusing is kept the temperature in this low-temperature melt, improve the recovery rate of rare earth Er；
(2) refining treatment, which uses, is free of MgCl2Dedicated refining agent, further reduced the scaling loss of rare earth Er in refining process；(3) originally
The heat treatment of the invention high-toughness heat-resistant casting Mg-Er alloy includes two processes of solution treatment and ageing treatment.Second level
480~490 DEG C, 36~48h of time of the first order temperature of solution treatment, the solubility of Er and Zn in magnesium matrix is sufficiently promoted,
Eliminate the coarse precipitated phases such as LPSO；535~545 DEG C, 1~2h of time of the first order temperature of second level solution treatment, short time heat preservation
Further eliminate the coarse phase such as undissolved LPSO, eliminate existing regional segregation, microsegregation in casting so that alloy at
Divide homogenization, to improve the performance of alloy, and prevents heat treatment burn-off phenomenon.Furnace temperature is maintained at 185~215 DEG C,
It keeps the temperature 12~36h and carries out ageing treatment, long period timeliness finally makes the transgranular precipitation Nano grade, dispersed and tiny reinforcing of alloy
Phase, so that alloy be made to have both excellent room temperature and high-temperature behavior.Heat treatment through the invention, alloying component are stablized, and crystal grain does not have
Have and obviously grow up, the performance of alloy is significantly improved, and method is simple, securely and reliably, easy to operate.
The present invention have it is following the utility model has the advantages that
High-toughness heat-resistant Mg-Er alloy suitable for gravitational casting of the invention is through gravitational casting, second level solution treatment and people
After work aging strengthening model, room temperature tensile intensity is 296MPa, elongation percentage 18%；Drawing by high temperature tensile strength is at 200 DEG C
215MPa, elongation percentage 23%, comprehensive performance reach the performance of cast aluminium alloy gold；Provided preparation method have simple process,
The advantages that high-efficient, suitable large-scale production, meet the high-end need that aerospace, military project, automobile and other industries develop lightweight
It asks.
Detailed description of the invention
Fig. 1 is the alloy microstructure figure prepared in embodiment 5.
Specific embodiment
Embodiment 1
The weight percent of high-toughness heat-resistant Mg-Er alloy suitable for gravitational casting are as follows: press stoichiometric, 6.0%Er,
4.2%Zn, 0.6%Al, 0.1%Mn, 0.08%Ti, surplus are Mg and other inevitable impurity.
Preparation method: (1) former needed for calculating by above-mentioned Mg-Er alloying component and stoichiometric ratio with due regard to after scaling loss
The dosage of material；Technical pure magnesium ingot, industrial-purity zinc, technical pure aluminium ingot and MgEr30 and MgMn10 intermediate alloy are removed into removing oxide layer
And it dries and is preheated to 200 DEG C.
(2) it after the technical pure magnesium ingot for accounting for crucible height 25% being fused into molten bath at 680 DEG C, is passed through containing 0.2% volume
The SF of score6And CO2Mixed gas, remaining magnesium ingot is added.
(3) after magnesium ingot all fusing, 700 DEG C are warming up to, by industrial-purity zinc and MgEr30 and MgMn10 intermediate alloy point 2
~4 additions, and keep temperature constant at 700 DEG C, it is stirred until all melting, and keep the temperature 30min.
(4) 40~60min before gravitational casting, is warming up to 730 DEG C, technical pure aluminium ingot to be sequentially added, AlTi5B1, AlB3
Intermediate alloy is all after fusing, and the refining agent that raw material weight 3.5% is added is refined, 730 DEG C of the temperature of refining, refining treatment
Mixing time 10min, refining agent component is by mass percentage are as follows: 55%KCl, 25%CaCl2, 5%CaF2, 15%BaCl2。
Furnace temperature is risen to 750 DEG C of heat preservations standings to promote within 10 minutes to be mingled with sedimentation, obtains magnesium alloy fused mass.
(5) magnesium alloy fused mass is cooled to 740 DEG C, skims surface scum, melt is poured by gravitational casting and is entered the room
In the sand mold type molds of 25 DEG C of temperature, the high-toughness heat-resistant casting Mg-Er alloy is obtained after cooling.
(6) second level solution treatment is successively carried out to resulting cast alloy, casting alloy is put into solid solution furnace, with 5 DEG C/
Min is warming up to 200 DEG C, is passed through the SF containing 0.2% volume fraction6And CO2Mixed gas, continue with 5 DEG C/min to be warming up to first
480 DEG C of solid solubility temperature of grade keeps the temperature 36h, is then warming up to 535 DEG C of second level solid solubility temperature at a slow speed with 10 DEG C/h, keeps the temperature fast after 1h
Speed, which is transferred on quenching unit, carries out water hardening.
(7) artificial aging processing is carried out to the casting alloy after solution treatment, quenched alloy is put into aging furnace,
185 DEG C of artificial aging treatment temperature are warming up to 5 DEG C/min, comes out of the stove after heat preservation 12h and is air-cooled to room temperature, obtains described be suitable for again
The high-toughness heat-resistant Mg-Er alloy of power casting.
High-toughness heat-resistant Mg-Er alloy obtained is subjected to a. room temperature tensile test respectively；B.200 DEG C, 200 hours heat is sudden and violent
In 200 DEG C of progress high temperature tensile properties tests after dew processing.The room temperature tensile for the high-toughness heat-resistant magnesium alloy that this example obtains is strong
Degree is 285MPa, elongation percentage 23%；Drawing by high temperature tensile strength is 203MPa, elongation percentage 28% at 200 DEG C.
Embodiment 2
The weight percent of high-toughness heat-resistant Mg-Er alloy suitable for gravitational casting are as follows: press stoichiometric, 4.0%Er,
2.0%Zn, 0.6%Al, 0.3%Mn, 0.01%Ti, 0.01%B, surplus are Mg and other inevitable impurity.
Preparation method: (1) former needed for calculating by above-mentioned Mg-Er alloying component and stoichiometric ratio with due regard to after scaling loss
The dosage of material；Technical pure magnesium ingot, industrial-purity zinc, technical pure aluminium ingot and MgEr30 and MgMn10 intermediate alloy are removed into removing oxide layer
And it dries and is preheated to 200 DEG C.
(2) after the technical pure magnesium ingot for accounting for crucible height 25% being fused into molten bath at 680 DEG C, it is passed through protective gas argon
Remaining magnesium ingot is added in gas.
(3) after magnesium ingot all fusing, 700 DEG C are warming up to, by industrial-purity zinc and MgEr30 and MgMn10 intermediate alloy point 2
~4 additions, and keep temperature constant at 700 DEG C, it is stirred until all melting, and keep the temperature 30min.
(4) 40~60min before gravitational casting, is warming up to 730 DEG C, technical pure aluminium ingot to be sequentially added, AlTi5 intermediate alloy
All after fusing, the refining agent that raw material weight 1% is added is refined, 730 DEG C of the temperature of refining, the mixing time of refining treatment
10min, refining agent component is by mass percentage are as follows: 55%KCl, 25%CaCl2, 5%CaF2, 15%BaCl2.Furnace temperature is risen to
750 DEG C of heat preservations stand 10 minutes and promote to be mingled with sedimentation, obtain magnesium alloy fused mass.
(5) magnesium alloy fused mass is cooled to 720 DEG C, skims surface scum, poured into melt by gravitational casting
It is preheated in 150 DEG C of sand mold type molds, the high-toughness heat-resistant casting Mg-Er alloy is obtained after cooling.
(6) second level solution treatment is successively carried out to resulting cast alloy, casting alloy is put into solid solution furnace, with 5 DEG C/
Min is warming up to 200 DEG C, is passed through protective gas argon gas, continues to be warming up to 490 DEG C of first order solid solubility temperature with 5 DEG C/min, heat preservation
Then 48h is warming up at a slow speed 545 DEG C of second level solid solubility temperature with 10 DEG C/h, fast transfer is enterprising to quenching unit after keeping the temperature 2h
Row water hardening.
(7) artificial aging processing is carried out to the casting alloy after solution treatment, quenched alloy is put into aging furnace,
215 DEG C of artificial aging treatment temperature are warming up to 5 DEG C/min, comes out of the stove after heat preservation 36h and is air-cooled to room temperature, obtains described be suitable for again
The high-toughness heat-resistant Mg-Er alloy of power casting.
High-toughness heat-resistant Mg-Er alloy obtained is subjected to a. room temperature tensile test respectively；B.200 DEG C, 200 hours heat is sudden and violent
In 200 DEG C of progress high temperature tensile properties tests after dew processing.The room temperature tensile for the high-toughness heat-resistant magnesium alloy that this example obtains is strong
Degree is 268MPa, elongation percentage 25%；Drawing by high temperature tensile strength is 185MPa, elongation percentage 33% at 200 DEG C.
Embodiment 3
The weight percent of high-toughness heat-resistant Mg-Er alloy suitable for gravitational casting are as follows: press stoichiometric, 10.0%Er,
2.0%Zn, 1.0%Al, 0.2%Mn, 0.05%Ti, 0.03%B, surplus are Mg and other inevitable impurity.
Preparation method: (1) former needed for calculating by above-mentioned Mg-Er alloying component and stoichiometric ratio with due regard to after scaling loss
The dosage of material；Technical pure magnesium ingot, industrial-purity zinc, technical pure aluminium ingot and MgEr30 and MgMn10 intermediate alloy are removed into removing oxide layer
And it dries and is preheated to 200 DEG C.
(2) after the technical pure magnesium ingot for accounting for crucible height 25% being fused into molten bath at 680 DEG C, it is passed through protective gas argon
Remaining magnesium ingot is added in gas.
(3) after magnesium ingot all fusing, 700 DEG C are warming up to, by industrial-purity zinc and MgEr30 and MgMn10 intermediate alloy point 2
~4 additions, and keep temperature constant at 700 DEG C, it is stirred until all melting, and keep the temperature 30min.
(4) 40~60min before gravitational casting, is warming up to 730 DEG C, in technical pure aluminium ingot to be sequentially added, AlTi10, AlB8
Between alloy all fusing after, be added raw material weight 2.5% refining agent refined, 720 DEG C of the temperature of refining, refining treatment
Mixing time 15min, refining agent component is by mass percentage are as follows: 55%KCl, 25%CaCl2, 5%CaF2, 15%BaCl2.It will
Furnace temperature rises to 750 DEG C of heat preservations standings and promotes within 10 minutes to be mingled with sedimentation, obtains magnesium alloy fused mass.
(5) magnesium alloy fused mass is cooled to 730 DEG C, skims surface scum, poured into melt by gravitational casting
It is preheated in 180 DEG C of metal type dies, the high-toughness heat-resistant casting Mg-Er alloy is obtained after cooling.
(6) second level solution treatment is successively carried out to resulting cast alloy, casting alloy is put into solid solution furnace, with 5 DEG C/
Min is warming up to 200 DEG C, is passed through protective gas argon gas, continues to be warming up to 485 DEG C of first order solid solubility temperature with 5 DEG C/min, heat preservation
Then 42h is warming up at a slow speed 540 DEG C of second level solid solubility temperature, after heat preservation 1.5h on fast transfer to quenching unit with 10 DEG C/h
Carry out water hardening.
(7) artificial aging processing is carried out to the casting alloy after solution treatment, quenched alloy is put into aging furnace,
200 DEG C of artificial aging treatment temperature are warming up to 5 DEG C/min, heat preservation is come out of the stove afterwards for 24 hours is air-cooled to room temperature, obtains described be suitable for again
The high-toughness heat-resistant Mg-Er alloy of power casting.
High-toughness heat-resistant Mg-Er alloy obtained is subjected to a. room temperature tensile test respectively；B.200 DEG C, 200 hours heat is sudden and violent
In 200 DEG C of progress high temperature tensile properties tests after dew processing.The room temperature tensile for the high-toughness heat-resistant magnesium alloy that this example obtains is strong
Degree is 290MPa, elongation percentage 22%；Drawing by high temperature tensile strength is 209MPa, elongation percentage 27% at 200 DEG C.
Embodiment 4
The weight percent of high-toughness heat-resistant Mg-Er alloy suitable for gravitational casting are as follows: press stoichiometric, 10.0%Er,
6.0%Zn, 1.2%Al, 0.2%Mn, 0.08%B, surplus are Mg and other inevitable impurity.
Preparation method: (1) former needed for calculating by above-mentioned Mg-Er alloying component and stoichiometric ratio with due regard to after scaling loss
The dosage of material；Technical pure magnesium ingot, industrial-purity zinc, technical pure aluminium ingot and MgEr30 and MgMn10 intermediate alloy are removed into removing oxide layer
And it dries and is preheated to 200 DEG C.
(2) it after the technical pure magnesium ingot for accounting for crucible height 25% being fused into molten bath at 680 DEG C, is passed through containing 0.2% volume
The SF of score6And CO2Hybrid protection gas, remaining magnesium ingot is added.
(3) after magnesium ingot all fusing, 700 DEG C are warming up to, by industrial-purity zinc and MgEr30 and MgMn10 intermediate alloy point 2
~4 additions, and keep temperature constant at 700 DEG C, it is stirred until all melting, and keep the temperature 30min.
(4) 40~60min before gravitational casting, is warming up to 730 DEG C, technical pure aluminium ingot to be sequentially added, AlB8 intermediate alloy
All after fusing, the refining agent that raw material weight 3.0% is added is refined, 720 DEG C of the temperature of refining, when the stirring of refining treatment
Between 15min, refining agent component is by mass percentage are as follows: 55%KCl, 25%CaCl2, 5%CaF2, 15%BaCl2.By furnace temperature liter
10 minutes are stood to 750 DEG C of heat preservations to promote to be mingled with sedimentation, obtain magnesium alloy fused mass.
(5) magnesium alloy fused mass is cooled to 720 DEG C, skims surface scum, poured into melt by gravitational casting
It is preheated in 250 DEG C of metal type dies, the high-toughness heat-resistant casting Mg-Er alloy is obtained after cooling.
(6) second level solution treatment is successively carried out to resulting cast alloy, casting alloy is put into solid solution furnace, with 5 DEG C/
Min is warming up to 200 DEG C, is passed through the SF containing 0.2% volume fraction6And CO2Hybrid protection gas, continuation be warming up to 5 DEG C/min
480 DEG C of first order solid solubility temperature, 48h is kept the temperature, is then warming up to 535 DEG C of second level solid solubility temperature at a slow speed with 10 DEG C/h, keeps the temperature 2h
Water hardening is carried out on fast transfer to quenching unit afterwards.
(7) artificial aging processing is carried out to the casting alloy after solution treatment, quenched alloy is put into aging furnace,
185 DEG C of artificial aging treatment temperature are warming up to 5 DEG C/min, comes out of the stove after heat preservation 36h and is air-cooled to room temperature, obtains described be suitable for again
The high-toughness heat-resistant Mg-Er alloy of power casting.
High-toughness heat-resistant Mg-Er alloy obtained is subjected to a. room temperature tensile test respectively；B.200 DEG C, 200 hours heat is sudden and violent
In 200 DEG C of progress high temperature tensile properties tests after dew processing.The room temperature tensile for the high-toughness heat-resistant magnesium alloy that this example obtains is strong
Degree is 296MPa, elongation percentage 18%；Drawing by high temperature tensile strength is 215MPa, elongation percentage 23% at 200 DEG C.
Embodiment 5
The weight percent of high-toughness heat-resistant Mg-Er alloy suitable for gravitational casting are as follows: press stoichiometric, 7.0%Er,
3.5%Zn, 0.5%Al, 0.3%Mn, 0.04%Ti, 0.04%B, surplus are Mg and other inevitable impurity.
Preparation method: (1) former needed for calculating by above-mentioned Mg-Er alloying component and stoichiometric ratio with due regard to after scaling loss
The dosage of material；Technical pure magnesium ingot, industrial-purity zinc, technical pure aluminium ingot and MgEr30 and MgMn10 intermediate alloy are removed into removing oxide layer
And it dries and is preheated to 200 DEG C.
(2) after the technical pure magnesium ingot for accounting for crucible height 25% being fused into molten bath at 680 DEG C, it is passed through protective gas argon
Remaining magnesium ingot is added in gas.
(3) after magnesium ingot all fusing, 700 DEG C are warming up to, by industrial-purity zinc and MgEr30 and MgMn10 intermediate alloy point 2
~4 additions, and keep temperature constant at 700 DEG C, it is stirred until all melting, and keep the temperature 30min.
(4) 40~60min before gravitational casting is warming up to 730 DEG C, to close among the technical pure aluminium ingot, AlTi5, AlB3
After gold is sequentially added and all melted, the refining agent that raw material weight 2.0% is added is refined, 730 DEG C of the temperature of refining, refining
The mixing time 10min of processing, refining agent component is by mass percentage are as follows: 55%KCl, 25%CaCl2, 5%CaF2, 15%
BaCl2.Furnace temperature is risen to 750 DEG C of heat preservations standings to promote within 10 minutes to be mingled with sedimentation, obtains magnesium alloy fused mass.
(5) magnesium alloy fused mass is cooled to 740 DEG C, skims surface scum, poured into melt by gravitational casting
It is preheated in 250 DEG C of metal type dies, the high-toughness heat-resistant casting Mg-Er alloy is obtained after cooling.
(6) second level solution treatment is successively carried out to resulting cast alloy, casting alloy is put into solid solution furnace, with 5 DEG C/
Min is warming up to 200 DEG C, is passed through the SF containing 0.2% volume fraction6And CO2Hybrid protection gas, continuation be warming up to 5 DEG C/min
490 DEG C of first order solid solubility temperature, 36h is kept the temperature, is then warming up to 545 DEG C of second level solid solubility temperature at a slow speed with 10 DEG C/h, keeps the temperature 1h
Water hardening is carried out on fast transfer to quenching unit afterwards.
(7) artificial aging processing is carried out to the casting alloy after solution treatment, quenched alloy is put into aging furnace,
215 DEG C of artificial aging treatment temperature are warming up to 5 DEG C/min, comes out of the stove after heat preservation 12h and is air-cooled to room temperature, obtains described be suitable for again
The high-toughness heat-resistant Mg-Er alloy of power casting.
High-toughness heat-resistant Mg-Er alloy obtained is subjected to a. room temperature tensile test respectively；B.200 DEG C, 200 hours heat is sudden and violent
In 200 DEG C of progress high temperature tensile properties tests after dew processing.The room temperature tensile for the high-toughness heat-resistant magnesium alloy that this example obtains is strong
Degree is 282MPa, elongation percentage 22%；Drawing by high temperature tensile strength is 197MPa, elongation percentage 26% at 200 DEG C.The present embodiment obtains
Magnesium alloy metallographic structure figure it is as shown in Figure 1.
Above-described embodiment is not limit the invention in any way, all to be obtained by the way of equivalent substitution or equivalent transformation
Technical solution fall within the scope of protection of the present invention.
Claims (13)
1. being suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting, it is characterised in that the element including following mass percent:
4.0~10.0%Er, 2.0~6.0%Zn, 0.5~1.2%Al, 0.1~0.3%Mn, 0.01~0.08%M, surplus be Mg and
Other inevitable impurity；Wherein, one or two kinds of in M Ti, B.
2. being suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting as described in claim 1, it is characterised in that: Zn/Er mass
Than being 0.2~0.7.
3. being suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting as described in claim 1, it is characterised in that: (Zn+Al)/
Er mass ratio is 0.3~0.8.
4. the preparation method of the high-toughness heat-resistant Mg-Er alloy as claimed in any one of claims 1 to 3 suitable for gravitational casting,
It is characterized by comprising following steps:
(1) Mg-Er alloying component and stoichiometric ratio are pressed, calculate technical pure magnesium ingot, industrial-purity zinc, technical pure aluminium ingot, in Mg-Er
Between alloy, Mg-Mn intermediate alloy, Al-Ti intermediate alloy, Al-Ti-B intermediate alloy and Al-B intermediate alloy dosage；It will be industrial
Pure magnesium ingot, industrial-purity zinc, technical pure aluminium ingot, Mg-Er intermediate alloy and Mg-Mn intermediate alloy remove removing oxide layer and dry preheating
To 200 DEG C；
(2) after the technical pure magnesium ingot for accounting for crucible height 25% being fused into molten bath, it is passed through protective gas, remaining magnesium ingot is added；
(3) after magnesium ingot all fusing, 700 DEG C are warming up to, by industrial-purity zinc, Mg-Er intermediate alloy and Mg-Mn intermediate alloy point
It is repeatedly added, and keeps temperature constant at 700 DEG C, be stirred until all melting, and keep the temperature 30min；
(4) 40~60min before gravitational casting, is warming up to 730 DEG C, technical pure aluminium ingot to be sequentially added, Al-Ti intermediate alloy,
Al-Ti-B intermediate alloy, Al-B intermediate alloy all after fusing, are added refining agent and are refined, furnace temperature is risen to 750 DEG C of heat preservations
10~20min is stood, promotion is mingled with sedimentation, obtains magnesium alloy fused mass；
(5) magnesium alloy fused mass is cooled between 720~740 DEG C and is removed the gred, poured into melt in advance by gravitational casting
In the sand mold type molds of heat to 25~150 DEG C or 180~250 DEG C of metal type dies, the high-toughness heat-resistant casting is obtained after cooling
Make Mg-Er alloy；
(6) second level solution treatment is successively carried out to resulting cast alloy, artificial aging processing obtains required high-toughness heat-resistant
Cast Mg-Er alloy.
5. the preparation method suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting, feature exist as claimed in claim 4
It is MgEr25 or MgEr30 in: the Mg-Er intermediate alloy, the Mg-Mn intermediate alloy is MgMn10, in the Al-Ti-B
Between alloy be AlTi5B1, the Al-B intermediate alloy be AlB3 or AlB8, the Al-Ti intermediate alloy be AlTi5 or
AlTi10。
6. the preparation method suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting, feature exist as claimed in claim 4
In: the mass percent component of the refining agent are as follows: 55%KCl, 25%CaCl2, 5%CaF2, 15%BaCl2。
7. the preparation method suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting, feature exist as claimed in claim 4
In: the refining agent additive amount is the 1.0~3.5% of raw material gross weight.
8. the preparation method suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting, feature exist as claimed in claim 4
In: refining temperature when refining agent refining is added is 720~730 DEG C, 10~15min of mixing time of refining treatment.
9. the preparation method suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting, feature exist as claimed in claim 4
In: the second level solid solution treatment process parameter are as follows: 480~490 DEG C of first order solid solubility temperature, 36~48h of soaking time；The second level
535~545 DEG C of solid solubility temperature, 1~2h of soaking time.
10. the preparation method suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting, feature exist as claimed in claim 9
In: the second level solid solution treatment process the step of are as follows: cast alloy is put into solid solution furnace, is warming up to 200 DEG C with 5 DEG C/min,
It is passed through protective gas, continues to be warming up to 480~490 DEG C of first order solid solubility temperature with 5 DEG C/min, keeps the temperature 36~48h；Then with 10
DEG C/h is warming up at a slow speed 535~545 DEG C of second level solid solution temperature, fast transfer is enterprising to quenching unit after keeping the temperature 1~2h
Row water hardening.
11. the preparation method of the high-toughness heat-resistant Mg-Er alloy suitable for gravitational casting as described in claim 4 or 10, special
Sign is: the SF that the protective gas is argon gas or volume fraction is 0.2%6And CO2Mixed gas.
12. the preparation method suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting, feature exist as claimed in claim 4
In: the artificial aging treatment process parameter: 185~215 DEG C of aging temp, 12~36h of soaking time.
13. the preparation method suitable for the high-toughness heat-resistant Mg-Er alloy of gravitational casting, feature exist as claimed in claim 12
In: the artificial aging treatment process the step of are as follows: quenched alloy is put into aging furnace, is warming up to people with 5 DEG C/min
It 185~215 DEG C of work aging temperature, comes out of the stove after keeping the temperature 12~36h and is air-cooled to room temperature.
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| CN102994834A (en) * | 2011-09-09 | 2013-03-27 | 江汉大学 | Heatproof magnesium alloy containing Nb |
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