CN109930045A - High-toughness heat-resistant Mg-Gd alloy and preparation method thereof suitable for gravitational casting - Google Patents
High-toughness heat-resistant Mg-Gd 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-Gd alloys and preparation method thereof for being suitable for gravitational casting, the alloy composition mass percentage content are as follows: 4.0~10.0%Gd, 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-Gd 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-Gd 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 300MPa, elongation percentage 15%；Drawing by high temperature tensile strength is 218MPa at 200 DEG C, and elongation percentage 20% meets the high demand that the industries such as aerospace, automobile, telecommunication develop lightweight.
Description
Technical field
The present invention relates to the high-toughness heat-resistant Mg-Gd 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 systems for the high-toughness heat-resistant Mg-Gd alloy for being suitable for gravitational casting
Preparation 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 (25wt%) of heavy rare earth element Gd in the magnesium alloy is very high, there is strong solution strengthening and ageing strengthening
Effect, addition Gd can greatly improve the compactness of magnesium alloy, casting character, three warm (low temperature, room temperature and high temperature) performances, resist it is compacted
Denaturation energy and corrosion resistance.It is found that early in researcher in 1974, by extruding, quenched and ageing treatment Mg-
15wt%Gd alloy is in high temperature and low temperature tensile strength all with higher.Although high Gd content leads to the density and cost of alloy
Increase, but researcher is dedicated to keeping the magnesium alloy containing gadolinium by coordinating addition alloy element such as Sc, Mn, Nd, Y, Zr
Mechanical property advantage reduces negative effect to the greatest extent, has developed some promising polynary magnesium alloys containing gadolinium, such as Mg-Gd-Y-
Mn, Mg-Gd-Y-Zr, Mg-Gd-Nd-Zr and Mg-Gd-Sc-Mn etc..
Cheap Zn is added in Mg-Gd alloy, not only the Precipitation group for regulating and controlling the alloy system is woven with more significant
Effect, and a variety of hardening constituents can be formed under the conditions of different Zn/Gd ratios: when mass ratio >=2.49 Zn/Gd in alloy
Icosahedral quasicrystal body structure I phase (Mg easy to form when (atomic ratio >=6.0)3Zn6Gd)；When in alloy Zn/Gd mass ratio between
Face-centred cubic structure W phase (Mg easy to form when (atomic ratio is between 1.5 and 6.0) between 0.62 and 2.493Zn3Gd2) and I phase；When
Zn/Gd mass ratio W phase easy to form and long period when (atomic ratio is between 1.0 and 1.5) between 0.42 and 0.62 in alloy
Stacking order structure LPSO phase (Mg12ZnGd)；It is easy to form when mass ratio≤0.42 Zn/Gd (atomic ratio≤1.0) in alloy
LPSO phase (Materials Science and Engineering A, 695 (2017) 135-143).A variety of Mg-Gd-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 CN105506426A
The change of more nanometers of phase complex intensifyings enhancing disclosed in sharp document (more nanometers of phase composite strengthening magnesium alloys of one kind and preparation method thereof)
Shape magnesium alloy, the quality percentage composition of the Mg-Gd-Zn alloy are as follows: 10~25%Gd, 1~5%Zn, surplus Mg, wherein Gd with
The mass percentage difference of Zn is not less than 8；Preparation method is to obtain one kind by classification extruding and multistage heat treatment process
The deformed magnesium alloy material of excellent in mechanical performance, the heat treatment temperature section are 200~550 DEG C, wherein solution treatment temperature
520~550 DEG C of section is spent, soaking time is 5~15h；450~520 DEG C for the treatment of temperature section is precipitated in high-temperature-phase, and soaking time is
10~120h；200~350 DEG C for the treatment of temperature section is precipitated in low-temperature phase, and soaking time is 15~100h.Application publication number is
The patent document (biodegradable Mg-Gd-Zn-Ag-Zr system magnesium alloy and preparation method thereof) of CN103184379A reports one
Kind biodegradable Mg-Gd-Zn-Ag-Zr system magnesium alloy and preparation method thereof, wherein the alloy is by Gd, Zn, Ag, Zr and Mg group
At the weight percentage of each component are as follows: 5~10%Gd, 0.5~3%Zn, 0.1~1%Ag, 0.1~1%Zr, surplus are
Mg.The preparation method of the alloy is the following steps are included: " (1) melting: the following raw material is added in smelting furnace and carries out melting: Gd is adopted
With Mg-Gd intermediate alloy, Zn uses pure zinc, and Ag uses fine silver, and Zr uses Mg-Zr intermediate alloy, and the Mg of surplus uses pure magnesium；On
Raw material is stated under protective gas after melting, is cast as Mg-Gd-Zn-Ag-Zr system magnesium alloy ingot；(2) Homogenization Treatments:
The Mg-Gd-Zn-Ag-Zr system magnesium alloy ingot that step (1) obtains is kept the temperature 6~24 hours at 480~550 DEG C；It (3) will be equal
The Mg-Gd-Zn-Ag-Zr system magnesium alloy that homogenizes that treated is squeezed or is rolled change after keeping the temperature 1~3 hour at 250~350 DEG C
Shape." foregoing invention are as follows: rare earth Gd content is too high to cause its density excessive, while expensive rare earth
Price causes the invention to be difficult industrially to be applied on a large scale.Alloy is thin although can carry out tissue by addition Zr
Change, but coarse grains under the conditions of conventional coagulation, and Mg-Gd-Zn precipitated phase is usually in coarse reticular structure, is deteriorated
Its mechanical property, it is necessary to which precipitate size is adjusted to play its hardening constituent by thermal deformation or heat treatment solid solution and timeliness
Effect.
Mg-Gd-Zn alloy is usually added into Zr as grain refining element, to refine its coarse microstructure.At present
Report adds Zr mode to have halogen, Zn-Zr intermediate alloy and Mg-Zr intermediate alloy of sponge Zr, Zr etc., wherein among Mg-Zr
Alloy have the advantages that it is easy to use, be mingled with less and good in refining effect, be the major way for being currently fed Zr.Such as: Shen Qing Publication
Number for a kind of patent document (high-strength heat-resistant magnesium alloy and preparation method thereof suitable for sand casting) of CN104928548A it is open
Mg-Gd-Y-Ag-Zr (B) magnesium-rare earth preparation method in by addition contain 0.2~0.6%Zr K2ZrF6Salt-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, the chemical activity of Zr is strong, at high temperature
It is easy to react with atmosphere, furnace gas, when using steel crucibles, when melt temperature is higher than 750 DEG C, Zr is easy and the Fe in crucible
Reaction, generates stable intermetallic compound Fe2Zr, the loss that these result in Zr are high；Many Zr in Mg-Zr intermediate alloy
It is to exist in the form of large scale simple substance Zr particle, since the fusing point of Zr is high (1852 DEG C), Zr particle is difficult to dissolve in melt,
In addition the density of Zr 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 be deposited 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
Gd alloy and preparation method thereof, for the alloy after gravitational casting is heat-treated, the room temperature tensile intensity of alloy is 300MPa, elongation percentage
15%；Drawing by high temperature tensile strength is 218MPa, elongation percentage 20% 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-Gd alloy of the present invention suitable for gravitational casting, the member including following mass percent
Element: 4.0~10.0%Gd, 2.0~6.0%Zn, 0.5~1.2%Al, 0.1~0.3%Mn, 0.01~0.08%M, surplus are
Mg and other inevitable impurity；Wherein, one or both of M Ti, B.
The innovative point of high-toughness heat-resistant Mg-Gd alloy provided by the invention suitable for 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 Gd is easy preparation because Gd has high corrosion resistance as its alloy element, the intermediate alloy of Mg-Gd.Alloying
Element Gd and Zn and matrix Mg element form ternary Mg-Gd-Zn hardening constituent.Especially in the model of Zn/Gd mass ratio 0.2~0.7
In enclosing, on the one hand, alloy of the present invention primarily forms long period stacking order structure LPSO phase (Mg12) and face-centred cubic structure ZnGd
W phase (Mg3Zn3Gd2), it is high-melting-point phase；With binary Mg-Gd hardening constituent ratio, ternary Mg-RE-Zn hardening constituent LPSO and W are in magnesium
High-temperature stable in matrix is more preferable, avoids the reduced performance as caused by precipitation strength phased soln, effectively enhances and is suitable for weight
The room-temperature mechanical property and high-temperature behavior of the high-toughness heat-resistant Mg-Gd alloy of power casting, especially room-temperature yield strength improve one
Times.On the other hand, the present invention solves traditional Mg-Zn-Gd alloy because excessively high Zn content causes freezing range excessive and easy
It generates thermal fragmentation defect, not can guarantee the toughness and tenacity of alloy and the technical problem of casting character.
(2) Mg-Gd-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 Gd 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-Gd-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.0.5-1.2%Al is added in alloy of the invention and substitutes Zr, forms disperse
High-melting-point Al2Gd phase has not only refined the tissue of alloy, but also the high temperature of Magnesium Alloy is ensured with high-temperature-phases such as LPSO
Stability.Al plays composite crystal grain fining together with a small amount of Ti and B simultaneously, has further refined alloy structure, has improved
The obdurability of alloy.A small amount of Mn is added in alloying element of the invention, can not only promote the formation of LPSO phase, improves alloy
High-temperature stability, and improve magnesium alloy corrosion resistance.
(3) in order to reduce the hot cracking tendency in Mg-Gd-Zn alloy casting process, Zn/Gd matter is limited in alloy of the invention
Amount is than 0.2~0.7 and (Zn+Al)/Gd 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-Gd-Zn alloy casting process
Performance.
The preparation method of the above-mentioned high-toughness heat-resistant Mg-Gd alloy suitable for gravitational casting, includes the following steps:
(1) with due regard to after scaling loss, by above-mentioned Mg-Gd alloying component and stoichiometric ratio, raw material (technical pure needed for calculating
Magnesium ingot, industrial-purity zinc, technical pure aluminium ingot, Mg-Gd intermediate alloy, Mg-Mn intermediate alloy, Al-Ti intermediate alloy, in Al-Ti-B
Between alloy and Al-B intermediate alloy) dosage；By technical pure magnesium ingot, industrial-purity zinc, technical pure aluminium ingot, Mg-Gd intermediate alloy and
Mg-Mn intermediate alloy removes removing oxide layer and dries to 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-Gd 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-Gd intermediate alloy is MgGd25 or MgGd30, 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 that perhaps the AlB8 Al-Ti intermediate alloy is AlTi5 or AlTi10 to AlB3.The refining agent
Mass percent component are as follows: 55%KCl, 25%CaCl2, 5%CaF2, 15%BaCl2.The refining agent additive amount is that raw material is total
The 1.0~3.5% of weight, refining temperature when refining agent refining is added are 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, obtains the high-toughness heat-resistant after cooling
Cast Mg-Gd alloy.
(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-Gd alloy.
The second level solutionizing step of high-toughness heat-resistant Mg-Gd alloy suitable for gravitational casting: cast alloy is put into solid
In molten furnace, 200 DEG C are warming up to 5 DEG C/min, being passed through protective gas, (protective gas is argon gas, or is containing volume fraction
0.2% SF6And CO2Mixed gas (i.e. SF6Volume fraction is 0.2%, CO2Volume fraction be 99.8%)), continue with 5
DEG C/min is warming up to 480~490 DEG C of first order solid solubility temperature, keep the temperature 36~48h；Then the second level is warming up at a slow speed with 10 DEG C/h
535~545 DEG C of solid solution temperature, water hardening is carried out on fast transfer to quenching unit after keeping the temperature 1~2h.
The artificial aging of high-toughness heat-resistant Mg-Gd alloy suitable for gravitational casting is handled, and the artificial aging handles work
The step of skill are as follows: quenched alloy is put into aging furnace, artificial aging treatment temperature 185~215 is warming up to 5 DEG C/min
DEG C, it comes out of the stove after 12~36h of heat preservation 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-Gd alloy provided by the invention suitable for gravitational casting: (1) exist
700 DEG C are added the Mg-Gd intermediate alloy of easy scaling loss, and fusing is kept the temperature in this low-temperature melt, improve the recovery rate of rare-earth Gd；
(2) refining treatment, which uses, is free of MgCl2Dedicated refining agent, further reduced the scaling loss of rare-earth Gd in refining process；(3) originally
The heat treatment of the invention high-toughness heat-resistant casting Mg-Gd 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 Gd 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-Gd 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 300MPa, elongation percentage 15%；Drawing by high temperature tensile strength is at 200 DEG C
218MPa, elongation percentage 20%, 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 obtained in embodiment 2.
Specific embodiment
Embodiment 1
The weight percent of high-toughness heat-resistant Mg-Gd alloy suitable for gravitational casting are as follows: press stoichiometric, 4.0%Gd,
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-Gd 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 MgGd30 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 MgGd30 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, among technical pure aluminium ingot to be sequentially added, AlTi10
Alloy, AlB3 intermediate alloy are all after fusing, and the refining agent that raw material weight 1% is added is refined, 730 DEG C of the temperature of refining,
The mixing time 10min of refining treatment, 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 720 DEG C, skims surface scum, melt is poured into 25 by gravitational casting
In the sand mold type molds of DEG C room temperature, the high-toughness heat-resistant casting Mg-Y 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-Y alloy of power casting.
High-toughness heat-resistant Mg-Gd 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 270MPa, elongation percentage 20%；Drawing by high temperature tensile strength is 188MPa, elongation percentage 31% at 200 DEG C.
Embodiment 2
The weight percent of high-toughness heat-resistant Mg-Gd alloy suitable for gravitational casting are as follows: press stoichiometric, 10.0%Gd,
6.0%Zn, 1.2%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-Gd 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 MgGd30 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 MgGd30 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, among technical pure aluminium ingot to be sequentially added, AlTi10
Alloy is all after fusing, and the refining agent that raw material weight 3.5% is added is refined, and 730 DEG C of the temperature of refining, refining treatment is stirred
Time 10min is mixed, refining agent component is by mass percentage are as follows: 55%KCl, 25%CaCl2, 5%CaF2, 15%BaCl2.By furnace
Temperature rise stands 10 minutes to 750 DEG C of heat preservations and promotes 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 215 DEG C of metal type dies, the high-toughness heat-resistant casting Mg-Y 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-Y alloy of power casting.
High-toughness heat-resistant Mg-Gd 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 300MPa, elongation percentage 15%；Drawing by high temperature tensile strength is 218MPa, elongation percentage 20% at 200 DEG C.The present embodiment obtains
Magnesium alloy cast metallographic structure figure it is as shown in Figure 1.
Embodiment 3
The weight percent of high-toughness heat-resistant Mg-Gd alloy suitable for gravitational casting are as follows: press stoichiometric, 7.0%Gd,
3.5%Zn, 0.5%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-Gd 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 MgGd30 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 MgGd30 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, among technical pure aluminium ingot to be sequentially added, AlTi5B1
Alloy, AlB3 intermediate alloy are all after fusing, and the refining agent that raw material weight 2.5% is added is refined, the temperature 720 of refining
DEG C, the mixing time 15min of refining treatment, 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 730 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-Y 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-Y alloy of power casting.
High-toughness heat-resistant Mg-Gd 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 17%；Drawing by high temperature tensile strength is 200MPa, elongation percentage 25% at 200 DEG C.
Embodiment 4
The weight percent of high-toughness heat-resistant Mg-Gd alloy suitable for gravitational casting are as follows: press stoichiometric, 6.0%Gd,
4.2%Zn, 0.6%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-Gd 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 MgGd30 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 MgGd30 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, closes among technical pure aluminium ingot to be sequentially added, AlB8
After golden all fusings, the refining agent that raw material weight 3.0% is added is refined, 720 DEG C of the temperature of refining, the stirring of refining treatment
Time 15min, refining agent component is by mass percentage are as follows: 55%KCl, 25%CaCl2, 5%CaF2, 15%BaCl2.By furnace temperature
It rises 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 720 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-Y 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-Y alloy of power casting.
High-toughness heat-resistant Mg-Gd 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 19%；Drawing by high temperature tensile strength is 207MPa, elongation percentage 27% at 200 DEG C.
Embodiment 5
The weight percent of high-toughness heat-resistant Mg-Gd alloy suitable for gravitational casting are as follows: press stoichiometric, 10.0%Gd,
2.0%Zn, 1.0%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-Gd 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 MgGd30 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 MgGd30 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, among technical pure aluminium ingot to be sequentially added, AlTi5B1
Alloy, AlB8 intermediate alloy are all after fusing, and the refining agent that raw material weight 2.0% is added is refined, the temperature 730 of refining
DEG C, the mixing time 10min of refining treatment, 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-Y 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-Y alloy of power casting.
High-toughness heat-resistant Mg-Gd 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 Mg-Gd alloy that this example obtains
Intensity is 296MPa, elongation percentage 18%；Drawing by high temperature tensile strength is 213MPa, elongation percentage 23% at 200 DEG C.
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-Gd alloy of gravitational casting, it is characterised in that the element including following mass percent:
4.0~10.0%Gd, 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-Gd alloy of gravitational casting as described in claim 1, it is characterised in that: Zn/Gd mass
Than being 0.2~0.7.
3. being suitable for the high-toughness heat-resistant Mg-Gd alloy of gravitational casting as described in claim 1, it is characterised in that: (Zn+Al)/
Gd mass ratio is 0.3~0.8.
4. the preparation method of the high-toughness heat-resistant Mg-Gd alloy as claimed in any one of claims 1 to 3 suitable for gravitational casting,
It is characterized by comprising following steps:
(1) Mg-Gd alloying component and stoichiometric ratio are pressed, calculate technical pure magnesium ingot, industrial-purity zinc, technical pure aluminium ingot, in Mg-Gd
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-Gd 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 is warming up to, industrial-purity zinc and Mg-Gd and Mg-Mn intermediate alloy are added several times
Enter, and keep temperature constant at 700 DEG C, 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, 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-Gd 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-Gd alloy.
5. the preparation method suitable for the high-toughness heat-resistant Mg-Gd alloy of gravitational casting, feature exist as claimed in claim 4
It is MgGd25 or MgGd30 in: the Mg-Gd 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-Gd 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-Gd 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-Gd 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-Gd 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-Gd 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-Gd 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-Gd 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-Gd 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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