CN108220729A - A kind of high-strength temperature-resistant cast magnesium alloy and preparation method thereof - Google Patents

A kind of high-strength temperature-resistant cast magnesium alloy and preparation method thereof Download PDF

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CN108220729A
CN108220729A CN201810148675.9A CN201810148675A CN108220729A CN 108220729 A CN108220729 A CN 108220729A CN 201810148675 A CN201810148675 A CN 201810148675A CN 108220729 A CN108220729 A CN 108220729A
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magnesium alloy
temperature
resistant cast
strength
cast magnesium
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谭何易
唐伦圆
胡军华
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Hunan Rong Tuo New Material Research Co Ltd
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Hunan Rong Tuo New Material Research Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon

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  • Crystallography & Structural Chemistry (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

The invention discloses a kind of high-strength temperature-resistant cast magnesium alloys and preparation method thereof, high-strength temperature-resistant cast magnesium alloy includes the nanometer Ti particles that mass percent is not more than 2%, and grain size≤850nm of nanometer Ti particles, the ingredient in high-strength temperature-resistant cast magnesium alloy include by mass percentage：Gd 4.0~9.0%；Y 2.5~4.5%；Zr 0.3~0.6%；Ti 0.2~1.6%；Surplus is Mg, other elements content summation≤0.2%；Wherein, Ti is nano particle, grain size≤800nm.The present invention uses high-strength temperature-resistant cast magnesium alloy, still has relatively excellent mechanical property under 300 DEG C of temperature conditions, at ambient temperature, tensile strength >=360Mpa, yield strength >=240Mpa, elongation percentage >=2.5%；Under 300 DEG C of temperature conditions, tensile strength >=240Mpa, yield strength >=150Mpa, elongation percentage >=8%.

Description

A kind of high-strength temperature-resistant cast magnesium alloy and preparation method thereof
Technical field
The present invention relates to a kind of high-strength temperature-resistant cast magnesium alloys and preparation method thereof, belong to field of new materials.
Background technology
Lightweight is equipment and parts manufacture eternal theme, and magnesium and magnesium alloy materials are current practical most light knots Structure metal material plays key player in lightweight process.Magnesium alloy has small (the about 1.8g/cm of density3), specific strength with Specific stiffness is big, damping vibration attenuation performance is good, capability of electromagnetic shielding is excellent, casting character is good and it is excellent to be easily recycled regeneration etc. Point is known as " the green structural metallic materials of 21 century most development and application potentiality ", be widely used in aerospace, The fields such as rail traffic, automobile, 3C industries and electric tool.And new-energy automobile has become the certainty of future automobile development at present Direction, this will provide new opportunity for the development of magnesium alloy.Magnesium alloy can be divided into cast magnesium alloy and deformation by molding mode Magnesium alloy, compared with wrought magnesium alloy, cast magnesium alloy has production efficiency height, manufacturing cost low and the complex-shaped work of easy processing The advantages that part, its market share is more than 80% at present, is the main molding mode of magnesium alloy.
However, routine casting magnesium alloy (such as AZ91D, AM60B, AZ31B) under normal temperature condition although have relatively excellent Different mechanical property, but when temperature is more than 120 DEG C, tensile strength dramatic decrease, poor high temperature stability, so as to limit casting Make the application of magnesium alloy materials mild high-temperature field in.Therefore, a kind of heat-resisting high-strength cast magnesium alloy is invented, is at present urgently Problem to be solved.
Titanium is a kind of silvery white transition metal, and large storage capacity, existence form are extensive, have it is light-weight, intensity is high, resistance to moist chlorine The features such as corrosion so that titanium becomes a current research hotspot.In order to improve the high-temperature behavior of magnesium alloy, except increasing rare earth Outside element, also sight has been turned on titanium elements.It, can after existing document record increases micro titanium elements in the magnesium alloy at present To improve the mechanical behavior under high temperature of magnesium alloy, but titanium elements can be used together with rare earth element, alkaline earth element under normal conditions, be reached To the effect of refining alloy tissue, and the general form for using intermediate alloy, it is added in alloy in melting process.(《Addition The influence of calcium and titanium to Mg-12Al-2Sr-0.3Mn Magnesium Alloys and performance》, volume 40 of mechanical engineering material 2 months 2016 2nd phase) but found during actually preparation and use, it is single use titanium valve and still mixes conduct with other elements Performance improvement element uses, and actual performance under the high temperature conditions is unable to reach requirement always, there are magnesium alloy hardness not The problems such as performance is unstable under up to standard or high temperature.
Invention content
In view of the above-mentioned problems existing in the prior art, the purpose of the present invention is obtain a kind of high-strength temperature-resistant cast magnesium alloy and Preparation method.
One of for achieving the above object, the technical solution of high-strength temperature-resistant cast magnesium alloy that the present invention uses is as follows：
The high-strength temperature-resistant cast magnesium alloy includes the nanometer Ti particles that mass percent is not more than 2%, and nanometer Ti Grain size≤850nm of grain.Not only the Ti elements with common grain size similarly improve performance under magnesium alloy high temperature to nanometer Ti particles Effect, and existing magnesium alloy hardness can be overcome low and high temperature under performance it is relatively low the problems such as.
Preferably, the high-strength heat-resistant magnesium alloy further includes rare earth Gd, Y and Zr, and surplus is magnesium in addition to impurity.
Preferably, the final alloy element of the high-strength temperature-resistant cast magnesium alloy includes by mass percentage：
Gd 4.0~9.0%；
Y 2.5~4.5%；
Zr 0.3~0.6%；
Ti 0.2~1.6%；And
Surplus is Mg, impurity content summation≤0.2%；
Wherein, Ti is nano particle, grain size≤800nm.
Other elements are member not to be covered in mixed said components in impurity inevitable in raw material or preparation process Element,
Its summation is no more than the 0.2% of magnesium alloy gross mass.The element proportioning of above-mentioned finished product is design value, but in practical inspection During survey,
There may be deviation, deviation ＜ 5% for the actual constituent of magnesium alloy made from it was found that.
Preferably, impurity element includes Si, Cu, Ni and Fe.Impurity element accounts for the gross mass degree point of total alloy It is not：Si≤0.05%, Cu≤0.025%, Ni≤0.001%, Fe≤0.004%.
Nanometer Ti particles serve not only as the nuclearing centre during material solidification, further promote uniformly dividing for other hardening constituents Cloth, therefore addition Ti nano particles can largely reduce the crystallite dimension of material.The Ti of common form due to grain size compared with Greatly, distributing homogeneity is poor and is only capable of making crystal enrichment molding as nucleation core, and molding magnesium alloy can not be protected at high temperature Good performance is held, but nanometer Ti particles (especially nanometer Ti particles are combined with rare-earth Gd and Y element) can ask to avoid this Topic, and tests prove that, nanometer Ti particles (especially nanometer Ti particles are combined with rare-earth Gd and Y element) are to the performance of magnesium alloy Raising is significantly improved under the conditions of 300 DEG C than other elements or nano particle.
The content of the Gd preferably accounts for the 7.0~8.0% of gross mass percentage.It can be seen from stretch test result Under equal conditions in claimed range, the content of Gd is higher, and the tensile strength and yield strength of magnesium alloy obtained are higher, and The variation tendency all maintained like under room temperature and 300 DEG C of high temperature.
The content of the Y preferably account for the 3.0~4.0% of gross mass percentage, it can be seen from stretch test result Under equal conditions in claimed range, the content of Y is higher, and the tensile strength and yield strength of magnesium alloy obtained are higher, extension Rate is also higher, and the variation tendency all maintained like under room temperature and 300 DEG C of high temperature.
The content of the Zr preferably accounts for the 0.4~0.5% of gross mass percentage.
The content of the Ti preferably accounts for the 0.6~1.0% of gross mass percentage.
As a kind of preferred embodiment, the ingredient of the high-strength heat-resistant magnesium alloy includes by mass percentage：
Gd 7.0~8.0%；
Y 3.0~4.0%；
Zr 0.4~0.5%；
Ti 0.6~1.0%；And
Surplus is Mg, impurity content summation≤0.2%；
Wherein, Ti is nano particle, grain size≤500nm.
Under equal conditions it can be seen from stretch test result in claimed range, the content of Ti is higher, magnesium obtained The tensile strength and yield strength of alloy are in gradual increased trend, and elongation percentage also more has identical raising trend, and in room temperature With the variation tendency all maintained like under 300 DEG C of high temperature.But inventor is it was unexpectedly observed that the content of Ti increases to one in an experiment Continue to increase after determining degree, the tensile strength and yield strength of magnesium alloy obtained have small size raising, but elongation percentage does not increase instead Drop, therefore, the raw material magnesium alloy combination of the content of Ti at 1.0% is a kind of embodiment party more preferred in the present invention Formula, the elongation percentage of the magnesium alloy of gained is best under this content, and more than 9.2% can be reached under the conditions of 300 DEG C.
Preferably, the particle size range of Ti nano particles is≤100nm.
As a preferred embodiment in the present invention, the element in magnesium alloy includes by mass percentage：Gd 7.0%th, Y 3.0%；Zr 0.4%；Grain size≤40nm of Ti 1.0%, Ti nano particle.
As a preferred embodiment in the present invention, element in the magnesium alloy is by mass percentage： Gd 7.5%, Y 3.5%；Zr 0.4%；Grain size≤80nm of Ti 1.1%, Ti nano particle.
Preferably, the raw material of the high-strength temperature-resistant cast magnesium alloy is selected from Mg-Gd intermediate alloys, Mg-Y intermediate alloys, Mg- Zr intermediate alloys and nanometer Ti particles.
Second object of the present invention is to provide a kind of preparation method of above-mentioned high-strength temperature-resistant cast magnesium alloy, the system Preparation Method first melts Mg-Gd intermediate alloys and Mg-Y intermediate alloys using two step fusion methods, remelted Mg-Zr intermediate alloys and receives Rice Ti particles.
Preferably, described method includes following steps：
A) pure magnesium melting：Bottom flux is added in into crucible, after crucible is dark red, adds in pure magnesium ingot fusing；
B) intermediate alloy melts：It is added among Mg-Gd intermediate alloys and Mg-Y into pure magnesium ingot after fusing obtained by step a) Alloy stirs evenly after fusing, adds Mg-Zr intermediate alloys and nanometer Ti particles, and the stirring of fishing bottom, must melt after melting again Alloy；
C) it refines：Refining agent is added into molten alloy obtained by step b), is stirred, slag is thoroughly dragged for and obtains molten alloy liquid；
D) heat preservation and composition detection：Molten alloy liquid obtained by step c), heat preservation stands and takes spectrum sample, if elemental composition It is up to standard, then carry out step e)；If elemental composition is not up to standard, step b) is returned to；
E) it casts：Molten alloy liquid up to standard in step d) is cast, obtains alloy pig.
Preferably, raw material preheating is further included before step a)：Raw material is weighed according to the percentage of component element and is carried out pre- Heat, wherein, 150~250 DEG C of preheating temperature, preheating time >=1h.
Preferably, the step f) being heat-treated to alloy pig is further included after step e)：Using T6 heat treatment process pair Alloy pig is heat-treated.
Preferably, step a) flux accounts for the 0.5~1.0% of melt gross mass.
Preferably, step b) melting temperatures are 730~780 DEG C.
Preferably, step c) refining temperatures are 740~760 DEG C, and refining agent is the 1%~2% of melt quality.
Preferably, step b) and step c) is stirred using argon gas and/or ultrasonic wave, mixing time >=10min.
Preferably, step d) holding temperatures are 780~800 DEG C, and soaking time is 20~30min.
Preferably, step e) cast temperatures are 710 DEG C~740 DEG C.
Preferably, 500~525 DEG C of step f) solid solubility temperatures, 6~12h of solution time；220~240 DEG C of aging temp, when Imitate 12~48h of time.
Preferably, bottom flux is RJ6 flux.
Preferably, step b) is melted for two steps, specially step b1) and b2)：
B1 the melting of Mg-Gd and Mg-Y intermediate alloys) is added in：When temperature reaches 730~740 DEG C, add among Mg-Gd and close Gold stirs after fusing；Mg-Y intermediate alloys are added, are stirred evenly after fusing；
B2) to step b1) Mg-Zr intermediate alloys and nanometer Ti particle fusions are added in gained melt：It is warming up to 760~ 780 DEG C, Mg-Zr intermediate alloys and nanometer Ti particles are added in, thoroughly drags for bottom stirring.
Preferably, Mg-Gd, Mg-Y, Mg-Zr intermediate alloy are respectively：It is closed among Mg-Gd containing gadolinium 30% (mass fraction) Gold, the Mg-Y intermediate alloys containing yttrium 30% (mass fraction), the Mg-Zr intermediate alloys containing zirconium 30% (mass fraction).
Following tissue change is substantially experienced during Mg-Gd-Y magnesium alloys solid solution aging：α-Mg+Mg5(Gd, Y) is common Crystalline phase → α-Mg+Mg5(Gd, Y) nodularization phase → α-Mg+Mg2Y3Gd2Square phase.The temperature and time of solid solution and timeliness and rare earth member The content of element is closely related.
Compared with prior art, high-strength temperature-resistant cast magnesium alloy of the invention still has phase under 300 DEG C of temperature conditions To excellent mechanical property, at ambient temperature, tensile strength >=360Mpa, yield strength >=240Mpa, elongation percentage >= 2.5%；Under 300 DEG C of temperature conditions, tensile strength >=240Mpa, yield strength >=150Mpa, elongation percentage >=8%；Addition is received Rice Ti particles can largely reduce the crystallite dimension of material, and the content of nanometer Ti particles is in 1wt%, 100nm or so When, magnesium alloy obtained is at ambient temperature or be optimal under the conditions of 300 DEG C.Easy to operate, the reflection of the present invention Time is short, suitable for industrial production, using with the close-fitting preparation process of rare earth element content, close the magnesium after Overheating Treatment Gold utensil has good mechanical property, and under the high temperature conditions, and the mechanical property range of decrease is smaller, has significant progress.Unexpected hair Existing optimal material combination has certain directive function, in of the invention for the magnesium alloy used under high temperature resistant environment Preparation process is environmental-friendly, raw material is cheap and easy to get, and dosage saving, has very big promotional value.
Specific embodiment
High-strength temperature-resistant cast magnesium alloy provided by the invention and preparation method thereof is made with reference to embodiment further detailed Carefully, completely illustrate.The embodiments described below is exemplary, and is only used for explaining the present invention, and it is not intended that this hair Bright limitation.
Experimental method in following embodiments is conventional method unless otherwise specified.It is real used in following embodiments It tests material unless otherwise specified, is that market is commercially available.
Tension test test is with reference to national standard GB/T 228.1-2010 in the embodiment of the present invention《Metal material stretching test the 1st Part：Room temperature test method》With GB/T 4330-2006《Metal Materials At High Temperature stretching test method》In related request.
Raw material in the embodiment of the present invention uses：In 99.95% pure magnesium ingot, the Mg-Gd containing gadolinium 30% (mass fraction) Between alloy, the Mg-Y intermediate alloys containing yttrium 30% (mass fraction), the Mg-Zr intermediate alloys containing zirconium 30% (mass fraction), contain The Mg-Ti intermediate alloys of titanium 10% (mass fraction), the Mg-Ca intermediate alloys of calcic 30% (mass fraction).Nanometer Ti particles (grain size≤800nm), nano SiC granule (grain size≤100nm).
First, embodiment
The constituent content of the magnesium alloy obtained in embodiment is as shown in table 1 below, and wherein constituent content is mass fraction, is removed Outside the component of each clear and definite content, surplus is magnesium, and other constituent content summation≤0.2%.Element proportioning in table 1 is design Value, but when actually detected, there may be deviation, deviation ＜ 5% for the actual constituent of magnesium alloy made from discovery.
1 embodiment constituent content table of table
The high-strength temperature-resistant cast magnesium alloy obtained in embodiment 1~11 is prepared in the following way：
It stocks up according to the constituent content in embodiment 1~11, the high-strength temperature-resistant cast magnesium alloy in the present embodiment Preparation method includes dispensing, raw material preheating, adds in pure magnesium melting, add in the melting of Mg-Gd and Mg-Y intermediate alloys, add in Mg-Zr Intermediate alloy and nanometer Ti particles simultaneously melt stirring, refining, heat preservation and composition detection, casting and heat treatment, specifically such as Under：
1) dispensing：Element proportioning and the proportion of goods damageds in above-described embodiment, calculate the addition needed for each raw material, And weigh the supplementary material of corresponding weight；
2) raw material preheating：The supplementary material weighed is preheated, 200 DEG C of preheating temperature, preheating time requirement 1h；
3) pure magnesium melting is added in：Appropriate RJ6 flux is added in into crucible as bottom flux, accounts for about the 0.5 of melt gross mass ~1.0%, after crucible is dark red, add in pure magnesium ingot；
4) melting of Mg-Gd and Mg-Y intermediate alloys is added in：When temperature reaches 730~740 DEG C, add among Mg-Gd and close Gold suitably stirs after fusing；When temperature rise to 730~740 DEG C again, Mg-Y intermediate alloys are added in, are suitably stirred after fusing, Make ingredient uniform；
5) Mg-Zr intermediate alloys and nanometer Ti particle fusions are added in：760~780 DEG C are warming up to, adds among Mg-Zr and closes Gold and nanometer Ti particles are thoroughly dragged for bottom stirring, are stirred using argon gas and ultrasonic wave, mixing time 10min；
6) it refines：Be cooled to 740~760 DEG C, start to refine, the additive amount of refining agent is 1%~2%, using argon gas and Ultrasonic wave stirs, and refining total time is 10min；
7) heat preservation and composition detection：Thoroughly fishing slag, and be warming up to 780~800 DEG C of 20~30min of heat preservation after the completion of refining, Spectrum sample is taken in insulating process, if elemental composition is up to standard, 710~740 DEG C is cooled to the furnace and waits for casting；If element into It is point not up to standard, then return to step 4) or 5)；
8) it casts：710 DEG C~740 DEG C are cooled to stove, is cast using metal pattern or sand mo(u)ld；
9) it is heat-treated：It is heat-treated using T6 techniques, 520 DEG C of solid solubility temperature, solution time 8h；220 DEG C of aging temp, Aging time is for 24 hours.
Treated, and high-strength heat-resistant magnesium alloy carries out stretching experiment, the results are shown in Table shown in 2.
2nd, comparative example
1. comparative example 1
The present embodiment uses the constituent content required in embodiment 3 to carry out molten refined after weighing raw material, and detailed process is such as Under：
1) dispensing：Element proportioning and the proportion of goods damageds in above-described embodiment, calculate the addition needed for each raw material, And weigh the supplementary material of corresponding weight；
2) raw material preheating：The supplementary material weighed is preheated, 200 DEG C of preheating temperature, preheating time requirement 1h；
3) pure magnesium melting is added in：Appropriate RJ6 flux is added in into crucible as bottom flux, accounts for about the 0.5 of melt gross mass ~1.0%, after crucible is dark red, add in pure magnesium ingot；
4) melting of Mg-Gd and Mg-Y intermediate alloys is added in：When temperature reaches 730~740 DEG C, add among Mg-Gd and close Gold suitably stirs after fusing；When temperature rise to 730~740 DEG C again, Mg-Y intermediate alloys are added in, are suitably stirred after fusing, Make ingredient uniform；
5) Mg-Zr intermediate alloys and nanometer Ti particle fusions are added in：760~780 DEG C are warming up to, adds among Mg-Zr and closes Gold and nanometer Ti particles thoroughly drag for bottom stirring, mechanical agitation 10min；
6) it refines：740~760 DEG C are cooled to, starts to refine, the additive amount of refining agent is 1%~2%, stirring refining 10min；
7) heat preservation and composition detection：Thoroughly fishing slag, and be warming up to 780~800 DEG C of 20~30min of heat preservation after the completion of refining, Spectrum sample is taken in insulating process, if elemental composition is up to standard, 710~740 DEG C is cooled to the furnace and waits for casting；If element into It is point not up to standard, then return to step 4) or 5)；
8) it casts：710 DEG C~740 DEG C are cooled to stove, is cast using metal pattern or sand mo(u)ld；
9) it is heat-treated：It is heat-treated using T6 techniques, 520 DEG C of solid solubility temperature, solution time 8h；220 DEG C of aging temp, Aging time is for 24 hours.
Treated, and high-strength heat-resistant magnesium alloy carries out stretching experiment, the results are shown in Table shown in 2.
2. comparative example 2
This comparative example using titaniferous 10% (mass fraction) source of the Mg-Ti intermediate alloys as Ti elements, prepare with Ti elements promote the high-strength temperature-resistant cast magnesium alloy of element for high-temperature behavior.The high-strength heat-resistant magnesium alloy of gained is each in the present embodiment Constituent content is as follows：Gd 7.0wt%, Y 3.0wt%, Zr 0.4wt%, Ti 1.0wt%, surplus is magnesium in addition to impurity.Specifically Preparation process it is as follows：
1) dispensing：Element proportioning and the proportion of goods damageds in above-described embodiment, calculate the addition needed for each raw material, And weigh the supplementary material of corresponding weight；
2) raw material preheating：The supplementary material weighed is preheated, 200 DEG C of preheating temperature, preheating time requirement 1h；
3) pure magnesium melting is added in：Appropriate RJ6 flux is added in into crucible as bottom flux, accounts for about the 0.5 of melt gross mass ~1.0%, after crucible is dark red, add in pure magnesium ingot；
4) melting of Mg-Gd and Mg-Y intermediate alloys is added in：When temperature reaches 730~740 DEG C, add among Mg-Gd and close Gold suitably stirs after fusing；When temperature rise to 730~740 DEG C again, Mg-Y intermediate alloys are added in, are suitably stirred after fusing, Make ingredient uniform；
5) Mg-Zr intermediate alloys and the melting of Mg-Ti intermediate alloys are added in：760~780 DEG C are warming up to, is added among Mg-Zr Alloy and Mg-Ti intermediate alloys are thoroughly dragged for bottom stirring, are stirred using argon gas and ultrasonic wave, mixing time 10min；
6) it refines：Be cooled to 740~760 DEG C, start to refine, the additive amount of refining agent is 1%~2%, using argon gas and Ultrasonic wave stirs, and refining total time is 10min；
7) heat preservation and composition detection：Thoroughly fishing slag, and be warming up to 780~800 DEG C of 20~30min of heat preservation after the completion of refining, Spectrum sample is taken in insulating process, if elemental composition is up to standard, 710~740 DEG C is cooled to the furnace and waits for casting；If element into It is point not up to standard, then return to step 4) or 5)；
8) it casts：710 DEG C~740 DEG C are cooled to stove, is cast using metal pattern or sand mo(u)ld；
9) it is heat-treated：It is heat-treated using T6 techniques, 520 DEG C of solid solubility temperature, solution time 8h；220 DEG C of aging temp, Aging time is for 24 hours.
Treated, and high-strength heat-resistant magnesium alloy carries out stretching experiment, the results are shown in Table shown in 2.
3. comparative example 3
This comparative example promotes material using nano SiC (grain size≤100nm) as high-temperature behavior, and what is prepared is high-strength resistance to The constituent content of hot cast magnesium alloy is as follows：Gd 7.0wt%, Y 3.0wt%, Zr 0.4wt%, SiC 1.0wt%, except impurity Outer surplus is magnesium.Specific preparation process is as follows：
1) dispensing：Element proportioning and the proportion of goods damageds in above-described embodiment, calculate the addition needed for each raw material, And weigh the supplementary material of corresponding weight；
2) raw material preheating：The supplementary material weighed is preheated, 200 DEG C of preheating temperature, preheating time requirement 1h；
3) pure magnesium melting is added in：Appropriate RJ6 flux is added in into crucible as bottom flux, accounts for about the 0.5 of melt gross mass ~1.0%, after crucible is dark red, add in pure magnesium ingot；
4) melting of Mg-Gd and Mg-Y intermediate alloys is added in：When temperature reaches 730~740 DEG C, add among Mg-Gd and close Gold suitably stirs after fusing；When temperature rise to 730~740 DEG C again, Mg-Y intermediate alloys are added in, are suitably stirred after fusing, Make ingredient uniform；
5) Mg-Zr intermediate alloys and nano SiC melting are added in：Be warming up to 760~780 DEG C, add in Mg-Zr intermediate alloys and Nano SiC is thoroughly dragged for bottom stirring, is stirred using argon gas and ultrasonic wave, mixing time 10min；
6) it refines：Be cooled to 740~760 DEG C, start to refine, the additive amount of refining agent is 1%~2%, using argon gas and Ultrasonic wave stirs, and refining total time is 10min；
7) heat preservation and composition detection：Thoroughly fishing slag, and be warming up to 780~800 DEG C of 20~30min of heat preservation after the completion of refining, Spectrum sample is taken in insulating process, if elemental composition is up to standard, 710~740 DEG C is cooled to the furnace and waits for casting；If element into It is point not up to standard, then return to step 4) or 5)；
8) it casts：710 DEG C~740 DEG C are cooled to stove, is cast using metal pattern or sand mo(u)ld；
9) it is heat-treated：It is heat-treated using T6 techniques, 520 DEG C of solid solubility temperature, solution time 8h；220 DEG C of aging temp, Aging time is for 24 hours.
Treated, and high-strength heat-resistant magnesium alloy carries out stretching experiment, the results are shown in Table shown in 2.
4. comparative example 4
This comparative example promotes element using Ca as high-temperature behavior, to be closed among the Mg-Ca of calcic 30% (mass fraction) Gold is used as raw material, and the magnesium alloy each element content of acquisition is as follows：Gd 7.0wt%, Y 3.0wt%, Zr 0.4wt%, Ca 1.0wt%, surplus is magnesium in addition to impurity.Specific preparation process is as follows：
1) dispensing：Element proportioning and the proportion of goods damageds in above-described embodiment, calculate the addition needed for each raw material, And weigh the supplementary material of corresponding weight；
2) raw material preheating：The supplementary material weighed is preheated, 200 DEG C of preheating temperature, preheating time requirement 1h；
3) pure magnesium melting is added in：Appropriate RJ6 flux is added in into crucible as bottom flux, accounts for about the 0.5 of melt gross mass ~1.0%, after crucible is dark red, add in pure magnesium ingot；
4) melting of Mg-Gd and Mg-Y intermediate alloys is added in：When temperature reaches 730~740 DEG C, add among Mg-Gd and close Gold suitably stirs after fusing；When temperature rise to 730~740 DEG C again, Mg-Y intermediate alloys are added in, are suitably stirred after fusing, Make ingredient uniform；
5) Mg-Zr intermediate alloys and the melting of Mg-Ca intermediate alloys are added in：760~780 DEG C are warming up to, is added among Mg-Zr Alloy and Mg-Ca intermediate alloys are thoroughly dragged for bottom stirring, are stirred using argon gas and ultrasonic wave, mixing time 10min；
6) it refines：Be cooled to 740~760 DEG C, start to refine, the additive amount of refining agent is 1%~2%, using argon gas and Ultrasonic wave stirs, and refining total time is 10min；
7) heat preservation and composition detection：Thoroughly fishing slag, and be warming up to 780~800 DEG C of 20~30min of heat preservation after the completion of refining, Spectrum sample is taken in insulating process, if elemental composition is up to standard, 710~740 DEG C is cooled to the furnace and waits for casting；If element into It is point not up to standard, then return to step 4) or 5)；
8) it casts：710 DEG C~740 DEG C are cooled to stove, is cast using metal pattern or sand mo(u)ld；
9) it is heat-treated：It is heat-treated using T6 techniques, 520 DEG C of solid solubility temperature, solution time 8h；220 DEG C of aging temp, Aging time is for 24 hours.
Treated, and high-strength heat-resistant magnesium alloy carries out stretching experiment, the results are shown in Table shown in 2.
5. comparative example 5
This comparative example uses Ti nano particles (grain size≤100nm) and titaniferous 10% (mass fraction) Mg-Ti intermediate alloys Source of the mixed raw material as Ti elements, prepare and the high-strength temperature-resistant of element is promoted using Ti elements as high-temperature behavior cast magnesium and close Gold.The high-strength heat-resistant magnesium alloy each element content of gained is as follows in the present embodiment：Gd 7.0wt%, Y 3.0wt%, Zr 0.4wt%, Ti 1.0wt%, wherein Ti nano particles and the ratio of amount containing Ti of Mg-Ti intermediate alloys are 1:1, the surplus in addition to impurity For magnesium.Specific preparation process is as follows：
1) dispensing：Element proportioning and the proportion of goods damageds in above-described embodiment, calculate the addition needed for each raw material, And weigh the supplementary material of corresponding weight；
2) raw material preheating：The supplementary material weighed is preheated, 200 DEG C of preheating temperature, preheating time requirement 1h；
3) pure magnesium melting is added in：Appropriate RJ6 flux is added in into crucible as bottom flux, accounts for about the 0.5 of melt gross mass ~1.0%, after crucible is dark red, add in pure magnesium ingot；
4) melting of Mg-Gd and Mg-Y intermediate alloys is added in：When temperature reaches 730~740 DEG C, add among Mg-Gd and close Gold suitably stirs after fusing；When temperature rise to 730~740 DEG C again, Mg-Y intermediate alloys are added in, are suitably stirred after fusing, Make ingredient uniform；
5) Mg-Zr intermediate alloys, Mg-Ti intermediate alloys and nanometer Ti particle fusions are added in：760~780 DEG C are warming up to, is added Enter Mg-Zr intermediate alloys, Mg-Ti intermediate alloys and nanometer Ti particles, thoroughly drag for bottom stirring, stirred using argon gas and ultrasonic wave, Mixing time 10min；
6) it refines：Be cooled to 740~760 DEG C, start to refine, the additive amount of refining agent is 1%~2%, using argon gas and Ultrasonic wave stirs, and refining total time is 10min；
7) heat preservation and composition detection：Thoroughly fishing slag, and be warming up to 780~800 DEG C of 20~30min of heat preservation after the completion of refining, Spectrum sample is taken in insulating process, if elemental composition is up to standard, 710~740 DEG C is cooled to the furnace and waits for casting；If element into It is point not up to standard, then return to step 4) or 5)；
8) it casts：710 DEG C~740 DEG C are cooled to stove, is cast using metal pattern or sand mo(u)ld；
9) it is heat-treated：It is heat-treated using T6 techniques, 520 DEG C of solid solubility temperature, solution time 8h；220 DEG C of aging temp, Aging time is for 24 hours.
Treated, and high-strength heat-resistant magnesium alloy carries out stretching experiment, the results are shown in Table shown in 2.
6. comparative example 6
This comparative example is using Ti nano particles (grain size≤100nm) with SiC nano particles (grain size≤100nm) as high temperature Performance boost material, the constituent content of the high-strength temperature-resistant cast magnesium alloy of acquisition are as follows：Gd 7.0wt%, Y 3.0wt%, Zr 0.4wt%, Ti 0.5wt%, SiC 0.5wt%, surplus is magnesium in addition to impurity.Specific preparation process is as follows：
1) dispensing：Element proportioning and the proportion of goods damageds in above-described embodiment, calculate the addition needed for each raw material, And weigh the supplementary material of corresponding weight；
2) raw material preheating：The supplementary material weighed is preheated, 200 DEG C of preheating temperature, preheating time requirement 1h；
3) pure magnesium melting is added in：Appropriate RJ6 flux is added in into crucible as bottom flux, accounts for about the 0.5 of melt gross mass ~1.0%, after crucible is dark red, add in pure magnesium ingot；
4) melting of Mg-Gd and Mg-Y intermediate alloys is added in：When temperature reaches 730~740 DEG C, add among Mg-Gd and close Gold suitably stirs after fusing；When temperature rise to 730~740 DEG C again, Mg-Y intermediate alloys are added in, are suitably stirred after fusing, Make ingredient uniform；
5) Mg-Zr intermediate alloys, nano SiC and nanometer Ti particle fusions are added in：760~780 DEG C are warming up to, adds in Mg- Zr intermediate alloys, nano SiC and nanometer Ti particles are thoroughly dragged for bottom stirring, are stirred using argon gas and ultrasonic wave, mixing time 10min；
6) it refines：Be cooled to 740~760 DEG C, start to refine, the additive amount of refining agent is 1%~2%, using argon gas and Ultrasonic wave stirs, and refining total time is 10min；
7) heat preservation and composition detection：Thoroughly fishing slag, and be warming up to 780~800 DEG C of 20~30min of heat preservation after the completion of refining, Spectrum sample is taken in insulating process, if elemental composition is up to standard, 710~740 DEG C is cooled to the furnace and waits for casting；If element into It is point not up to standard, then return to step 4) or 5)；
8) it casts：710 DEG C~740 DEG C are cooled to stove, is cast using metal pattern or sand mo(u)ld；
9) it is heat-treated：It is heat-treated using T6 techniques, 520 DEG C of solid solubility temperature, solution time 8h；220 DEG C of aging temp, Aging time is for 24 hours.
Treated, and high-strength heat-resistant magnesium alloy carries out stretching experiment, the results are shown in Table shown in 2.
7. comparative example 7
This comparative example is mixed with Ca elements using nanometer Ti particles (grain size≤100nm) and promotes element as high-temperature behavior, Using the Mg-Ca intermediate alloys of calcic 30% (mass fraction) as the source of Ca elements, the high-strength temperature-resistant cast magnesium alloy of acquisition Constituent content it is as follows：Gd 7.0wt%, Y 3.0wt%, Zr 0.4wt%, Ti 0.5wt%, Ca 0.5wt%, in addition to impurity Surplus is magnesium.Specific preparation process is as follows：
1) dispensing：Element proportioning and the proportion of goods damageds in above-described embodiment, calculate the addition needed for each raw material, And weigh the supplementary material of corresponding weight；
2) raw material preheating：The supplementary material weighed is preheated, 200 DEG C of preheating temperature, preheating time requirement 1h；
3) pure magnesium melting is added in：Appropriate RJ6 flux is added in into crucible as bottom flux, accounts for about the 0.5 of melt gross mass ~1.0%, after crucible is dark red, add in pure magnesium ingot；
4) melting of Mg-Gd and Mg-Y intermediate alloys is added in：When temperature reaches 730~740 DEG C, add among Mg-Gd and close Gold suitably stirs after fusing；When temperature rise to 730~740 DEG C again, Mg-Y intermediate alloys are added in, are suitably stirred after fusing, Make ingredient uniform；
5) Mg-Zr intermediate alloys and nanometer Ti particle fusions are added in：760~780 DEG C are warming up to, adds among Mg-Zr and closes Gold and nanometer Ti particles are thoroughly dragged for bottom stirring, are stirred using argon gas and ultrasonic wave, mixing time 10min；
6) it refines：Be cooled to 740~760 DEG C, start to refine, the additive amount of refining agent is 1%~2%, using argon gas and Ultrasonic wave stirs, and refining total time is 10min；
7) heat preservation and composition detection：Thoroughly fishing slag, and be warming up to 780~800 DEG C of 20~30min of heat preservation after the completion of refining, Spectrum sample is taken in insulating process, if elemental composition is up to standard, 710~740 DEG C is cooled to the furnace and waits for casting；If element into It is point not up to standard, then return to step 4) or 5)；
8) it casts：710 DEG C~740 DEG C are cooled to stove, is cast using metal pattern or sand mo(u)ld；
9) it is heat-treated：It is heat-treated using T6 techniques, 520 DEG C of solid solubility temperature, solution time 8h；220 DEG C of aging temp, Aging time is for 24 hours.
Treated, and high-strength heat-resistant magnesium alloy carries out stretching experiment, the results are shown in Table shown in 2.
2 embodiment tension test tables of data of table
By Tables 1 and 2 it is found that the present invention magnesium alloy at high temperature, mechanical property still maintains a good state, and embodiment Component proportion in 3 has apparent synergistic effect, and mechanical property has larger advantage.Conventional AZ91D magnesium alloy room temperature Under the conditions of, tensile strength be 220~260Mpa, 160~180Mpa of yield strength, elongation percentage 6~8%；AZ91D magnesium alloys are super 150 DEG C are crossed, intensity drastically declines, such as under the conditions of 300 DEG C, tensile strength ＜ 80Mpa, yield strength ＜ 60Mpa, substantially Failure.High-strength temperature-resistant cast magnesium alloy in the present invention at ambient temperature, tensile strength >=360Mpa, yield strength >= 240Mpa, elongation percentage >=2.5%；Under 300 DEG C of temperature conditions, tensile strength >=240Mpa, yield strength >=150Mpa, extension Rate >=8%.
For the particle of nanometer Ti shown in Examples 1 to 4 when grain size is identical, content is bigger in room temperature and 300 DEG C of items in magnesium alloy Tensile strength and yield strength under part is bigger, illustrates that magnesium alloy is not only greatly improved in height in a nanometer addition for Ti particles Intensive parameter under temperature, and it is proportional between the content and intensive parameter of Ti elements.But according to elongation percentage pair of one Than finding that nanometer Ti particles elongation percentage in 1% content is best, the overall target of magnesium alloy is preferably also, and increase content is extremely The growth rate when growth rate of parameters is less than 1% compared with Ti contents when 1.5% is declined, therefore can rationally calculate cashier When rice Ti particles are near mass percent is 1%, the magnesium alloy of acquisition is at normal temperatures best with the performance parameter under high temperature Range.
The comparison of embodiment 3,5,6,7 understands the smaller magnesium alloy of grain size of nanometer Ti particles under the conditions of room temperature and 300 DEG C Performance is better, but by grain size it can be seen from embodiment 3 and 5 40nm is down to by 100nm after parameters growth rate under Drop, therefore consider with reference to cost, 100nm is most preferred particle size range.Embodiment 8 and 10, embodiment 9 and 11 two groups of comparisons Understand that tensile strength and the yield strength of the higher magnesium alloy of rare earth Gd content are higher；Embodiment 8 and 9, embodiment 10 and 11 Two groups of comparisons understand that the tensile strength of the higher magnesium alloy of rare earth element y content and yield strength are higher；But compare Gd elements and Y members It finds that experimental result is unstable on elongation percentage after element, illustrates that the two is little or not directly proportional for the contribution of elongation percentage, tool Body conclusion needs further to prove by microscopic structure.
The difference of comparative example 1 and embodiment 3 is the difference of preparation process, and embodiment 3 is equal in melting and refinement step It is stirred using ultrasonic wave, each raw material is made fully to spread, crystal grain distribution is more uniform and stable after molten refined, therefore under similary component Properties of Magnesium Alloy it is more excellent.
In the experimental data of comparative example 2,3,4, although being added to rare earth element, using Mg-Ti alloys, nano SiC or The nanometer Ti particles that Mg-Ca alloys can not be substituted in the present invention are played substantially change Properties of Magnesium Alloy under 300 DEG C of high temperature Effect, the Ti elements of other forms or other conventional use of nano particles be unable to reach nanometer Ti particles to magnesium alloy height The promotion effect of warm nature energy.Comparative example 5~7 promotes material using the mixing of nanometer Ti particles and above-mentioned material as high-temperature behavior, Although the magnesium alloy in acquisition increases in performance, due to the decline of nanometer Ti granule contents, the degree of performance raising Also declined, when exclusive use nanometer Ti particles can not also be realized by further proving the mixing of other materials and nanometer Ti particles Promotion effect.
It is it is necessary to described herein finally：Above example is served only for making technical scheme of the present invention further detailed Ground explanation, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art's the above according to the present invention Some the nonessential modifications and adaptations made all belong to the scope of protection of the present invention.

Claims (10)

1. a kind of high-strength temperature-resistant cast magnesium alloy, which is characterized in that the high-strength temperature-resistant cast magnesium alloy includes quality percentage Than the nanometer Ti particles for being not more than 2%, and grain size≤850nm of nanometer Ti particles.
2. high-strength temperature-resistant cast magnesium alloy according to claim 1, which is characterized in that the high-strength heat-resistant magnesium alloy into Divide and include by mass percentage：
Gd 4.0~9.0%；
Y 2.5~4.5%；
Zr 0.3~0.6%；
Ti 0.2~1.6%；And
Surplus is Mg, impurity content summation≤0.2%；
Wherein, Ti is nano particle, grain size≤800nm.
3. high-strength temperature-resistant cast magnesium alloy according to claim 1, it is characterised in that：Impurity element include Si, Cu, Ni and Fe。
4. high-strength temperature-resistant cast magnesium alloy according to claim 1, it is characterised in that：The content of the Gd accounts for gross mass hundred Divide the 7.0~8.0% of ratio.
5. high-strength temperature-resistant cast magnesium alloy according to claim 1, it is characterised in that：The content of the Y accounts for gross mass hundred Divide the 3.0~4.0% of ratio.
6. high-strength temperature-resistant cast magnesium alloy according to claim 1, it is characterised in that：The content of the Zr accounts for gross mass hundred Divide the 0.4~0.5% of ratio.
7. high-strength temperature-resistant cast magnesium alloy according to claim 1, it is characterised in that：The content of the Ti accounts for gross mass hundred Divide the 0.6~1.0% of ratio.
8. high-strength temperature-resistant cast magnesium alloy according to claim 1, it is characterised in that：The particle size range of Ti nano particles is ≤500nm。
9. a kind of prepare such as the preparation method of claim 1~8 any one of them high-strength temperature-resistant cast magnesium alloy, feature exists Mg-Gd intermediate alloys and Mg-Y intermediate alloys are first melted using two step fusion methods, in, the preparation method in remelted Mg-Zr Between alloy and nanometer Ti particles.
10. the preparation method of high-strength temperature-resistant cast magnesium alloy according to claim 9, it is characterised in that：The preparation side Method includes the following steps：
A) pure magnesium melting：Bottom flux is added in into crucible, after crucible is dark red, adds in pure magnesium ingot；
B) intermediate alloy melts：Mg-Gd intermediate alloys and Mg-Y intermediate alloys are added in into pure magnesium ingot after fusing obtained by step a), It is stirred evenly after fusing, adds Mg-Zr intermediate alloys and nanometer Ti particles, the stirring of fishing bottom, obtains molten alloy after melting again；
C) it refines：Refining agent is added into molten alloy obtained by step b), is stirred, slag is thoroughly dragged for and obtains molten alloy liquid；
D) heat preservation and composition detection：Molten alloy liquid obtained by step c), heat preservation stands and takes spectrum sample, if elemental composition reaches Mark, then carry out step e)；If elemental composition is not up to standard, step b) is returned to；
E) it casts：Molten alloy liquid up to standard in step d) is cast, obtains alloy pig.
CN201810148675.9A 2018-02-13 2018-02-13 A kind of high-strength temperature-resistant cast magnesium alloy and preparation method thereof Pending CN108220729A (en)

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