CN113337765A - High-temperature and high-pressure creep-resistant die-casting magnesium alloy and preparation method thereof - Google Patents
High-temperature and high-pressure creep-resistant die-casting magnesium alloy and preparation method thereof Download PDFInfo
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- 238000004512 die casting Methods 0.000 title claims abstract description 102
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 131
- 239000000956 alloy Substances 0.000 claims abstract description 131
- 239000011777 magnesium Substances 0.000 claims abstract description 50
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 48
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 44
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 26
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 24
- 239000012535 impurity Substances 0.000 claims abstract description 17
- 239000011701 zinc Substances 0.000 claims description 63
- 239000007788 liquid Substances 0.000 claims description 45
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 37
- 238000002156 mixing Methods 0.000 claims description 26
- 239000011572 manganese Substances 0.000 claims description 23
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 238000005266 casting Methods 0.000 claims description 21
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 20
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 19
- 229910052748 manganese Inorganic materials 0.000 claims description 17
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 16
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 229910052726 zirconium Inorganic materials 0.000 claims description 15
- 238000003723 Smelting Methods 0.000 claims description 12
- 230000001681 protective effect Effects 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 5
- 239000013078 crystal Substances 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 230000002045 lasting effect Effects 0.000 abstract description 4
- 238000012795 verification Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 22
- MIOQWPPQVGUZFD-UHFFFAOYSA-N magnesium yttrium Chemical compound [Mg].[Y] MIOQWPPQVGUZFD-UHFFFAOYSA-N 0.000 description 18
- RIAXXCZORHQTQD-UHFFFAOYSA-N lanthanum magnesium Chemical compound [Mg].[La] RIAXXCZORHQTQD-UHFFFAOYSA-N 0.000 description 17
- 238000001514 detection method Methods 0.000 description 14
- 229910052802 copper Inorganic materials 0.000 description 9
- 229910052742 iron Inorganic materials 0.000 description 9
- 229910052759 nickel Inorganic materials 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 238000002347 injection Methods 0.000 description 8
- 239000007924 injection Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000000155 melt Substances 0.000 description 8
- 239000007769 metal material Substances 0.000 description 8
- 238000010998 test method Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000005275 alloying Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- KBMLJKBBKGNETC-UHFFFAOYSA-N magnesium manganese Chemical compound [Mg].[Mn] KBMLJKBBKGNETC-UHFFFAOYSA-N 0.000 description 5
- QRNPTSGPQSOPQK-UHFFFAOYSA-N magnesium zirconium Chemical compound [Mg].[Zr] QRNPTSGPQSOPQK-UHFFFAOYSA-N 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910052790 beryllium Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000013016 damping Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910018137 Al-Zn Inorganic materials 0.000 description 1
- 229910018573 Al—Zn Inorganic materials 0.000 description 1
- 241000219312 Chenopodium Species 0.000 description 1
- 229910003023 Mg-Al Inorganic materials 0.000 description 1
- JTUZZGLMVUXHQL-UHFFFAOYSA-N [Y].[Sm] Chemical compound [Y].[Sm] JTUZZGLMVUXHQL-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000013079 quasicrystal Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
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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
- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
- B22D17/08—Cold chamber machines, i.e. with unheated press chamber into which molten metal is ladled
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Continuous Casting (AREA)
Abstract
A high temperature and high pressure creep resistant die-casting magnesium alloy and a preparation method thereof belong to the technical field of magnesium alloy. Solves the problem that the creep resistance of the magnesium alloy in the prior art can not completely meet the use requirement under the environment of more than 200 ℃. The magnesium alloy of the present invention comprises: 1-6 wt% of Zn, 0.5-4 wt% of La, 0.5-6 wt% of Y, 0-0.5 wt% of Zr, 0-0.5 wt% of Mn, and the balance of magnesium and inevitable impurity elements. The magnesium alloy contains Zn, La and Y, the three components form a continuous reticular second phase structure distributed in three-dimensional space after being melted, the second phase has a plurality of structures simultaneously, thereby effectively hindering dislocation slippage and twin crystal formation under the high temperature condition, improving the high temperature creep resistance of the alloy,proved by verification, the creep stress is 80MPa at 250 ℃, the lasting creep life is more than 300h, and the steady-state creep rate is less than 6 multiplied by 10‑9/s。
Description
Technical Field
The invention belongs to the technical field of magnesium alloy, and particularly relates to a high-temperature and high-pressure creep-resistant die-casting magnesium alloy and a preparation method thereof.
Background
The magnesium alloy is formed by adding other elements into magnesium as a base, and has the characteristics of low density, high specific strength, high specific rigidity, good damping and vibration damping performance, good electromagnetic shielding performance, excellent casting and machining performance and the like. Therefore, the method has important application value and wide application prospect in the fields of automobiles, 3C, aerospace, national defense, military industry and the like.
In the prior art, the most applied magnesium alloy is die-casting magnesium alloy, and an alloy system mainly focuses on AZ (Mg-Al-Zn) magnesium alloy and AM (Mg-Al-Mn) magnesium alloy; however, the creep-cast magnesium alloy with the two systems has poor performance of resisting high temperature and high pressure, and the use temperature is strictly limited below 120 ℃. Since key power transmission parts have high requirements on the heat resistance of materials, in order to promote the application of magnesium alloys in power transmission parts, a great deal of researchers begin to pay attention to heat-resistant and creep-resistant magnesium alloys, and successfully develop AE (Mg-AL-RE) series, AS (Mg-Al-Si) series, Mg-Al-Ca series and Mg-Al-Sr series magnesium alloys, which have good heat resistance and can be used at a temperature of 175 ℃, wherein the use temperature of the AE44 alloy can be close to 200 ℃. However, the heat-resistant and creep-resistant magnesium alloy developed at present is rarely applied, and the main reason for the application is that the high-temperature and high-pressure creep resistance can not meet the actual use requirements, such as the use requirements that the use temperature is more than 250 ℃ and the stress is more than 70 MPa. Therefore, the development of high temperature and high pressure creep resistant magnesium alloys has become a necessary trend in the development of heat resistant magnesium alloys.
In the prior art, a die-casting magnesium alloy with better high-temperature and high-pressure creep resistance is developed by adding rare earth elements, alkaline earth elements and the like into Mg-Al series alloy, but when the temperature is higher than 200 ℃, the creep resistance of the alloy is sharply reduced, and even at 200 ℃, the creep strength of the alloy is generally lower than 70 MPa. Further alloying of the AE alloy significantly improves the high-temperature strength of the alloy, but significantly reduces the creep resistance of the alloy. Therefore, the creep resistance of the magnesium alloy in the prior art can not completely meet the use requirement under the environment of 200 ℃ and above.
Disclosure of Invention
The invention aims to provide a high-temperature and high-pressure creep resistant die-casting magnesium alloy which can be used at 250 ℃, has the creep strength of more than 120MPa at 200 ℃ and is more than 80MPa at 250 ℃.
The technical scheme adopted by the invention for realizing the aim is as follows.
The invention provides a high-temperature and high-pressure creep resistant die-casting magnesium alloy, which comprises the following components:
1 to 6 wt% of zinc (Zn), 0.5 to 4 wt% of lanthanum (La), 0.5 to 6 wt% of yttrium (Y), 0 to 0.5 wt% of zirconium (Zr), 0 to 0.5 wt% of manganese (Mn), and the balance of magnesium and unavoidable impurity elements.
Preferably, the mass content of Zn is 3% to 5%.
Preferably, the La is 1.5 to 3% by mass.
Preferably, the mass content of Y is 2.5-4.5 wt%
The invention also provides a preparation method of the high-temperature and high-pressure creep resistant die-casting magnesium alloy, which comprises the following steps:
1) taking a magnesium source, a zinc source, a lanthanum source, an yttrium source, a zirconium source and a manganese source according to the composition, and smelting to obtain an alloy liquid;
2) and (2) carrying out high-pressure casting on the alloy liquid obtained in the step 1) to obtain the high-temperature and high-pressure creep-resistant die-casting magnesium alloy.
Preferably, in the step 1), the melting temperature is 700 ℃ to 760 ℃.
Preferably, in the step 1), smelting is carried out under the condition of protective gas, and the volume ratio of the protective gas to SF is 1 (50-120)6And CO2。
Preferably, in the step 1), the magnesium source, the zinc source, the lanthanum source, the yttrium source, the zirconium source and the manganese source are preheated before being smelted, and the preheating temperature is 180-400 ℃.
Preferably, the step 1) is:
1a) taking a magnesium source, a zinc source, a lanthanum source, an yttrium source, a zirconium source and a manganese source according to the composition;
1b) smelting a magnesium source, a lanthanum source and an yttrium source to obtain a first mixed molten metal;
1c) mixing a zirconium source, a manganese source and the first mixed molten metal obtained in the step 1b) to obtain a second mixed molten metal;
1d) and mixing the second mixed metal liquid with a zinc source to obtain alloy liquid.
More preferably, in the step 1c), the mixing time of the zirconium source, the manganese source and the first mixed metal solution is 5min to 10min, the mixing temperature is 720 ℃ to 750 ℃, and in the step 1d), the mixing time of the second mixed metal solution and the zinc source is 8min to 20 min.
Preferably, in the step 2), before the alloy liquid is subjected to high-pressure casting, the alloy liquid is kept stand for 20-45 min, and the temperature of the alloy liquid is 700-720 ℃ during standing.
Preferably, the high-pressure casting in the step 2) is casting by a cold chamber die casting machine, and the temperature of a die-casting melt is 700-730 ℃; the preheating temperature of the die-casting die is 180-300 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the high-temperature and high-pressure resistant creep die-casting magnesium alloy contains Zn, La and Y, and the Zn, the La and the Y form second-phase grids which are formed by a plurality of crystal structures and are continuously distributed in a three-dimensional space after being melted, and the second-phase space network structures can effectively hinder dislocation slippage and twin crystal formation under a high-temperature condition, so that the resistance of alloy deformation is improved; in addition, Zn and Y in the magnesium matrix of the alloy can form basal plane precipitated phases in the creep process, thereby effectively hindering basal plane dislocation slippage; therefore, the alloy provided by the invention has extremely excellent high-temperature and high-pressure creep resistance. The test proves that: the high-temperature and high-pressure creep resistant die-casting magnesium alloy has the creep stress of 120MPa at 200 ℃, the lasting creep life of more than 500h and the steady-state creep rate of less than 1 multiplied by 10-9S; at 250 ℃, the creep stress is 80MPa, the lasting creep life is more than 300h, and the steady state creep rate is less than 6 multiplied by 10-9And/s is superior to commercial AE44 and Mg-Al-Ca, Mg-Al-Sr and Mg-Al-Si series alloys.
The preparation method of the high-temperature and high-pressure resistant creeping pressure casting magnesium alloy provided by the invention is safe and reliable, simple in process and low in cost.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a metallographic structure photograph of a high temperature and high pressure creep resistant die-cast magnesium alloy obtained in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of the die-cast magnesium alloy with high temperature and high pressure creep resistance obtained in example 1 of the present invention.
Detailed Description
For a further understanding of the invention, preferred embodiments of the invention are described below in conjunction with the detailed description, but it is to be understood that the description is intended to further illustrate the features and advantages of the invention and not to limit the claims to the invention.
The invention relates to a high-temperature and high-pressure creep resistant die-casting magnesium alloy, which comprises the following components: 1-6 wt% of Zn, 0.5-4 wt% of La, 0.5-6 wt% of Y, 0-0.5 wt% of Zr, 0-0.5 wt% of Mn, and the balance of Mg and inevitable impurity elements (if impurity elements can be avoided, the impurity elements are not contained).
The high-temperature-resistant high-pressure-resistant creeping pressure casting magnesium alloy provided by the invention comprises 1-6 wt% of Zn. In the present invention, the mass content of Zn in the high temperature and high pressure creep resistant die-cast magnesium alloy is preferably 3% to 5%, and most preferably 4%. The content of Zn in the high-temperature and high-pressure creep-resistant die-casting magnesium alloy provided by the invention ensures that a high-temperature and high-pressure creep-resistant die-casting magnesium alloy melt has very good flowing property, and further the high-temperature and high-pressure creep-resistant die-casting magnesium alloy can be used for preparing a casting with a complex structure by a die-casting method.
The high-temperature-resistant high-pressure-resistant creep-deformation casting magnesium alloy provided by the invention comprises 0.5-4 wt% of La. In the present invention, the content by mass of La in the die-cast magnesium alloy resistant to high-temperature and high-pressure creep is preferably 1.5% to 3%, and most preferably 3%. In the invention, La can act together with Zn in the technical scheme to further improve the fluidity of the alloy liquid and inhibit the hot cracking behavior of the alloy in the die-casting process, so that the high-temperature and high-pressure resistant creep-deformation casting magnesium alloy provided by the invention has better casting quality.
The high-temperature-resistant high-pressure-resistant creeping pressure casting magnesium alloy comprises 0.5-6 wt% of Y. In the invention, the mass content of Y in the high-temperature and high-pressure creep-resistant die-casting magnesium alloy is preferably 2.5-4.5%, and most preferably 3.5%. In the invention, Y can be combined with Zn and matrix Mg in the technical scheme to form a ternary phase, wherein the ternary phase also comprises a ternary long-range periodic phase and a quasicrystal phase, and the ternary phases are alternately distributed to form a continuous grid structure in spatial distribution.
The high-temperature-resistant high-pressure-resistant creep-casting magnesium alloy provided by the invention can also comprise other alloy elements, such as 0-0.5 wt% of Zr and 0-0.5 wt% of Mn, in the invention, the other alloy elements do not obviously influence the high-temperature-resistant high-pressure-creep property of the alloy, but the crystal grains of the alloy can be refined to a certain extent by adding Zr, and the content of impurity elements such as Fe in the alloy can be reduced by adding Mn. Therefore, the high-temperature and high-pressure creep resistant die-casting magnesium alloy provided by the invention has more excellent corrosion resistance and the like.
The high-temperature and high-pressure creep resistant die-casting magnesium alloy provided by the invention has the inevitable impurity elements of one or more of Si, Fe, Ni, Cu, Be and the like, and the total amount of the impurity elements is less than 0.1 wt%.
The preparation method of the high-temperature and high-pressure resistant creeping pressure casting magnesium alloy comprises the following steps:
1) taking a magnesium source, a zinc source, a lanthanum source, an yttrium source, a zirconium source and a manganese source according to the composition, and smelting to obtain an alloy liquid;
2) and (2) carrying out high-pressure casting on the alloy liquid obtained in the step 1) to obtain the high-temperature and high-pressure creep-resistant die-casting magnesium alloy.
The smelting method is not particularly limited in the invention, and the technical scheme of metal smelting known to those skilled in the art can be adopted.
The smelting temperature is preferably 700-760 ℃, more preferably 720-740 ℃, and most preferably 730 ℃.
The invention preferably carries out smelting under the condition of protective gas; the present invention is not particularly limited in kind and source of the protective gas, and the protective gas used in the preparation of the magnesium alloy, which is well known to those skilled in the art, may be used and may be commercially available. In the present invention, the protective gas is preferably SF6And CO2；SF6And CO2The volume ratio of (A) to (B) is preferably 1 (50-120), and most preferably 1: 80.
In the present invention, the melting is preferably carried out under stirring conditions, and the stirring speed is not particularly limited.
When the high-temperature and high-pressure resistant creep-deformation casting magnesium alloy does not contain other alloy elements, the magnesium source, the lanthanum source and the yttrium source are preferably smelted to obtain a first mixed molten metal; and then mixing the first mixed molten metal and a zinc source to obtain alloy liquid. The mixing time of the first mixed metal solution and the zinc source is preferably 8min to 20min, more preferably 10min to 15 min.
When the high-temperature and high-pressure creep-resistant die-casting magnesium alloy contains other alloy elements, the magnesium source, the lanthanum source and the yttrium source are preferably smelted to obtain a first mixed molten metal; then mixing the first mixed molten metal with other alloy elements (one or two of a zirconium source and a manganese source) to obtain a second mixed molten metal; and finally, mixing the second mixed molten metal with a zinc source to obtain alloy liquid. In the present invention, the mixing temperature of the first mixed molten metal and the source of the other alloying element is preferably 720 ℃ to 750 ℃, more preferably 725 ℃ to 740 ℃, and most preferably 730 ℃. In the present invention, the mixing time of the first mixed molten metal and the other alloying elements is preferably 5 to 10min, and more preferably 6 to 8 min. The mixing time of the second mixed metal solution and the zinc source is preferably 8min to 20min, and more preferably 10min to 15 min.
In the present invention, the magnesium source, the zinc source, the lanthanum source, the yttrium source, the zirconium source, and the manganese source are preferably preheated before they are melted. In the present invention, the temperature at which the magnesium, zinc, lanthanum, yttrium, zirconium and manganese sources are preheated is preferably 180 to 400 ℃, more preferably 240 to 360 ℃, and most preferably 300 ℃.
In the present invention, the zinc source is preferably pure zinc. In the present invention, the magnesium source is preferably pure magnesium. The present invention is not particularly limited in the source of zinc source and magnesium source, and can be commercially available. In the present invention, the lanthanum source is preferably a magnesium-lanthanum master alloy. In the invention, the mass fraction of lanthanum in the magnesium-lanthanum intermediate alloy is preferably 15-40%, and more preferably 20-30%. In the present invention, the yttrium source is preferably a magnesium-yttrium master alloy. In the invention, the mass fraction of yttrium in the magnesium-yttrium master alloy is preferably 15-40%, and more preferably 20-30%. The source of lanthanum and yttrium sources is not particularly limited in the present invention and may be any of the above-mentioned sources known to those skilled in the art and commercially available. In the present invention, the other alloying element source is preferably a magnesium-other alloying element master alloy, such as a magnesium-zirconium master alloy, a magnesium-manganese master alloy. In the invention, the mass fractions of other alloy elements in the magnesium-other alloy element intermediate alloy are not particularly limited, and the alloy preparation conditions can be met. The source of the other alloying element sources is not particularly limited in the present invention, and any source of the above kind known to those skilled in the art may be used, and may be commercially available.
In the present invention, after the alloy liquid is obtained, argon gas may be introduced into the alloy liquid to refine the alloy liquid. In the present invention, it is preferable not to refine. In the present invention, the alloy liquid is preferably left to stand. In the invention, the standing time is preferably 20 min-45 min, and the melt temperature during standing is preferably 700-720 ℃.
The alloy liquid of the invention is preferably cast at high pressure by a cold chamber die casting machine to obtain the high-temperature and high-pressure creep resistant die casting magnesium alloy. In the present invention, the die casting melt temperature is preferably 700 ℃ to 730 ℃, more preferably 705 ℃ to 720 ℃, and most preferably 710 ℃ to 720 ℃. In the invention, the die-casting injection rate is not particularly limited, and the quality of the die-casting sample can be ensured by adopting the technical scheme of magnesium alloy die-casting, which is well known to a person skilled in the art. The preheating temperature of the die-casting die is preferably 180-300 ℃, more preferably 220-270 ℃, and most preferably 240-260 ℃.
The high-temperature and high-pressure resistant creep die-casting magnesium alloy contains Zn, La and Y, and the Zn, the La and the Y form second-phase grids which are formed by a plurality of crystal structures and are continuously distributed in a three-dimensional space after being melted, and the second-phase space network structures can effectively hinder dislocation slippage and twin crystal formation under a high-temperature condition, so that the resistance of alloy deformation is improved; in addition, Zn and Y in the magnesium matrix of the alloy can form basal plane precipitated phases in the creep process, thereby effectively hindering basal plane dislocation slippage; therefore, the alloy provided by the invention has extremely excellent high-temperature and high-pressure creep resistance.
The invention can control the dosage of magnesium source, zinc source, lanthanum source and yttrium source (and other alloy element sources) to obtain the high temperature and high pressure creep resistance of the alloy.
The creep property of the high-temperature and high-pressure resistant creep-deformation casting magnesium alloy provided by the invention at high temperature is tested according to the standard of GB/T2039-2012 'Metal Material uniaxial tension creep test method'. The experimental result is that the creep stress is 120MPa at 200 ℃, the lasting creep life is more than 500h, and the creep rate is less than 5 multiplied by 10-10S; at 250 deg.C, creep stress is 80MPa, endurance creep life is greater than 300h, creep rate is less than 6X 10-9/s。
For further understanding of the present invention, the creep-cast magnesium alloy with high temperature and high pressure resistance and the preparation method thereof provided by the present invention are described in detail below with reference to the examples, but they should not be construed as limiting the scope of the present invention.
The raw materials used in the following examples of the present invention are all commercially available products, and the lanthanum source, yttrium source and other alloying element sources are respectively magnesium-lanthanum intermediate alloy, magnesium-yttrium intermediate alloy, magnesium-manganese intermediate alloy and magnesium-zirconium intermediate alloy provided by libanite magnesium corporation, chenopodium. The mass fraction of lanthanum in the magnesium-lanthanum intermediate alloy is 20%, the mass fraction of yttrium samarium in the magnesium-yttrium intermediate alloy is 20%, the mass fraction of manganese in the magnesium-manganese intermediate alloy is 4%, the mass fraction of zirconium in the magnesium-zirconium intermediate alloy is 33%, and the zinc is pure zinc.
Example 1
10650g of pure magnesium, 600g of pure zinc and 500g of magnesium were mixed togetherLanthanum master alloy, 2250g of magnesium-yttrium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium, magnesium lanthanum intermediate alloy and magnesium yttrium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2The volume ratio of the mixed gas to the mixed gas is 1:80, after the materials are melted, the melt is heated to 730 ℃, and then the pure zinc preheated to 300 ℃ is added into a crucible under the stirring condition for mixing for 8min to obtain alloy liquid; and cooling the alloy liquid to 715 ℃, and standing for 30 min.
And die-casting the alloy liquid after standing on a cold chamber die casting machine with 280 tons of mold clamping force to obtain the high-temperature and high-pressure creep-resistant die-casting magnesium alloy, wherein the die-casting temperature is 715 ℃, the die-casting mold temperature is 240 +/-20 ℃, and the injection speed of die-casting is 2 m/s.
The high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 1 of the invention is subjected to component detection by using a spectrum analyzer, and the detection result shows that the high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 1 of the invention comprises the following components: 3.88 wt% of Zn, 2.01 wt% of La, 2.95 wt% of Y, less than 0.1 wt% of the total amount of impurity elements Fe, Cu, Si and Ni, and the balance of magnesium. The optical photograph and the scanning photograph of the creep deformation resistant magnesium alloy obtained in the embodiment 1 of the present invention are observed, and the observation results are respectively shown in fig. 1 and fig. 2. It can be seen that the gas structure of the high-temperature and high-pressure resistant creep-deformation casting magnesium alloy obtained in the embodiment 1 of the invention is fine and uniform, and a continuous second-phase space grid structure is formed.
And testing the high-temperature and high-pressure creep resistance of the alloy according to the standard of GB/T2039-2012 'test method for uniaxial tensile creep of metal materials'. The experimental result shows that the creep life is more than 500h at 200 ℃ and 120MPa, and the creep rate is less than 1 multiplied by 10-9S; at 250 deg.C, creep stress is 80MPa, endurance creep life is greater than 300h, creep rate is less than 6X 10-9/s。
Example 2
11475g of pure magnesium, 150g of pure zinc, 3000g of magnesium-lanthanum master alloy, 375g of magnesium-yttrium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium, magnesium lanthanum intermediate alloy and magnesium yttrium intermediate alloy into a crucible preheated to 300 ℃,introducing SF into the crucible6And CO2The volume ratio of the mixed gas to the mixed gas is 1:80, after the materials are melted, the melt is heated to 730 ℃, and then the pure zinc preheated to 300 ℃ is added into a crucible under the stirring condition for mixing for 8min to obtain alloy liquid; and cooling the alloy liquid to 715 ℃, and standing for 30 min.
And die-casting the alloy liquid after standing on a cold chamber die casting machine with 280 tons of mold clamping force to obtain the high-temperature and high-pressure creep-resistant die-casting magnesium alloy, wherein the die-casting temperature is 715 ℃, the die-casting mold temperature is 240 +/-20 ℃, and the injection speed of die-casting is 2 m/s.
The high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 2 of the invention is subjected to component detection by using a spectrum analyzer, and the detection result shows that the high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 2 of the invention comprises the following components: 1.06 wt% of Zn, 3.82 wt% of La, 0.43 wt% of Y, less than 0.1 wt% of the total amount of impurity elements Fe, Cu, Si and Ni, and the balance of magnesium.
And testing the high-temperature and high-pressure creep resistance of the alloy according to the standard of GB/T2039-2012 'test method for uniaxial tensile creep of metal materials'. The experimental result shows that the creep life is more than 500h at 200 ℃ and 100MPa, and the creep rate is less than 1 multiplied by 10-9/s。
Example 3
9600g of pure magnesium, 900g of pure zinc, 3000g of magnesium-lanthanum master alloy, 500g of magnesium-yttrium master alloy are preheated to 180 ℃. Firstly, putting preheated pure magnesium, magnesium lanthanum intermediate alloy and magnesium yttrium intermediate alloy into a crucible preheated to 180 ℃, and introducing SF into the crucible6And CO2The volume ratio of the mixed gas to the mixed gas is 1:80, after the materials are melted, the melt is heated to 720 ℃, and then the pure zinc preheated to 180 ℃ is added into a crucible under the stirring condition for mixing for 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 30 min.
And die-casting the alloy liquid after standing on a cold chamber die casting machine with 280 tons of mold clamping force to obtain the high-temperature and high-pressure creep-resistant die-casting magnesium alloy, wherein the die-casting temperature is 710 ℃, the die-casting mold temperature is 240 +/-20 ℃, and the injection speed of die-casting is 2 m/s.
The high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 3 of the invention is subjected to component detection by using a spectrum analyzer, and the detection result shows that the high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 3 of the invention comprises the following components: 5.95 wt% of Zn, 4.03 wt% of La, 1.99 wt% of Y, less than 0.1 wt% of the total amount of impurity elements Fe, Cu, Si and Ni, and the balance of magnesium.
And testing the high-temperature and high-pressure creep resistance of the alloy according to the standard of GB/T2039-2012 'test method for uniaxial tensile creep of metal materials'. The experimental result shows that the creep rate at 200 ℃ and 100MPa is less than 1 multiplied by 10-9/s。
Example 4
9525g of pure magnesium, 600g of pure zinc, 375g of magnesium lanthanum master alloy, 4500g of magnesium yttrium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium, magnesium lanthanum intermediate alloy and magnesium yttrium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2The volume ratio of the mixed gas to the mixed gas is 1:80, after the materials are melted, the melt is heated to 750 ℃, and then the pure zinc preheated to 300 ℃ is added into a crucible under the stirring condition for mixing for 8min to obtain alloy liquid; and cooling the alloy liquid to 730 ℃, and standing for 30 min.
And die-casting the alloy liquid after standing on a 280-ton mold clamping force cold chamber die-casting machine to obtain the high-temperature and high-pressure creep-resistant die-casting magnesium alloy, wherein the die-casting temperature is 730 ℃, the die-casting mold temperature is 240 +/-20 ℃, and the injection speed of die-casting is 2 m/s.
The high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 4 of the invention is subjected to component detection by using a spectrum analyzer, and the detection result shows that the high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 4 of the invention comprises the following components: 3.97 wt% of Zn, 0.50 wt% of La, 5.72 wt% of Y, less than 0.1 wt% of the total amount of impurity elements Fe, Cu, Si and Ni, and the balance of magnesium.
And testing the high-temperature and high-pressure creep resistance of the alloy according to the standard of GB/T2039-2012 'test method for uniaxial tensile creep of metal materials'. The experimental result shows that the creep rate at 200 ℃ and 120MPa is less than 1 multiplied by 10-9/s。
Example 5
9750g of pure magnesium, 375g of pure zinc, 1875g of magnesium lanthanum master alloy, 3000g of magnesium yttrium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium, magnesium lanthanum intermediate alloy and magnesium yttrium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2The volume ratio of the mixed gas to the mixed gas is 1:80, after the materials are melted, the melt is heated to 730 ℃, and then the pure zinc preheated to 300 ℃ is added into a crucible under the stirring condition for mixing for 8min to obtain alloy liquid; and cooling the alloy liquid to 700 ℃, and standing for 30 min.
And die-casting the alloy liquid after standing on a cold chamber die casting machine with 280 tons of die locking force to obtain the high-temperature and high-pressure creep-resistant die-casting magnesium alloy, wherein the die-casting temperature is 700 ℃, the die-casting die temperature is 180 +/-20 ℃, and the injection speed of die-casting is 2 m/s.
The high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 5 of the invention is subjected to component detection by using a spectrum analyzer, and the detection result shows that the high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 5 of the invention comprises the following components: 2.47 wt% of Zn, 2.36 wt% of La, 3.91 wt% of Y, less than 0.1 wt% of the total amount of impurity elements Fe, Cu, Si and Ni, and the balance of magnesium.
And testing the high-temperature and high-pressure creep resistance of the alloy according to the standard of GB/T2039-2012 'test method for uniaxial tensile creep of metal materials'. The experimental result shows that the creep rate at 200 ℃ and 120MPa is less than 1 multiplied by 10-9/s。
Example 6
8775g of pure magnesium, 600g of pure zinc, 150g of magnesium-lanthanum master alloy, 2250g of magnesium-yttrium master alloy and 1875g of magnesium-manganese master alloy were preheated to 400 ℃. Firstly, putting preheated pure magnesium, magnesium lanthanum intermediate alloy and magnesium yttrium intermediate alloy into a crucible preheated to 400 ℃, and introducing SF into the crucible6And CO2The volume ratio of the mixed gas to the mixed gas is 1:80, the melt is heated to 730 ℃ after the materials are melted, then the magnesium-manganese intermediate alloy preheated to 400 ℃ is added into a crucible under the stirring condition for mixing for 8min, and then the pure zinc preheated to 400 ℃ is added for mixing for 8minMixing to obtain alloy liquid; and cooling the alloy liquid to 715 ℃, and standing for 30 min.
And die-casting the alloy liquid after standing on a cold chamber die casting machine with 280 tons of die locking force to obtain the high-temperature and high-pressure creep-resistant die-casting magnesium alloy, wherein the die-casting temperature is 715 ℃, the die-casting die temperature is 300 +/-20 ℃, and the injection speed of die-casting is 2 m/s.
The high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 6 of the invention is subjected to component detection by using a spectrum analyzer, and the detection result shows that the high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 6 of the invention comprises the following components: 3.92 wt% of Zn, 1.98 wt% of La, 3.01 wt% of Y, 0.37 wt% of Mn, less than 0.1 wt% of the total amount of impurity elements Fe, Cu, Si and Ni, and the balance of magnesium.
And testing the high-temperature and high-pressure creep resistance of the alloy according to the standard of GB/T2039-2012 'test method for uniaxial tensile creep of metal materials'. The experimental result shows that the creep rate at 200 ℃ and 120MPa is less than 1 multiplied by 10-9/s。
Example 7
9950g of pure magnesium, 600g of pure zinc, 500g of magnesium lanthanum master alloy, 2250g of magnesium yttrium master alloy and 700g of magnesium zirconium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium, magnesium lanthanum intermediate alloy and magnesium yttrium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2The volume ratio of the mixed gas to the mixed gas is 1:80, the melt is heated to 720 ℃ after the materials are melted, then the magnesium-zirconium intermediate alloy preheated to 300 ℃ is added into a crucible under the stirring condition for mixing for 8min, and then the pure zinc preheated to 300 ℃ is added for mixing for 8min to obtain alloy liquid; and cooling the alloy liquid to 715 ℃, and standing for 30 min.
And die-casting the alloy liquid after standing on a 280-ton mold clamping force cold chamber die-casting machine to obtain the high-temperature and high-pressure creep-resistant die-casting magnesium alloy, wherein the die-casting temperature is 715 ℃, the die-casting mold temperature is 280 +/-20 ℃, and the injection speed of die-casting is 2 m/s.
The high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 7 of the invention is subjected to component detection by using a spectrum analyzer, and the detection result shows that the high-temperature and high-pressure creep-resistant die-casting magnesium alloy obtained in the embodiment 7 of the invention comprises the following components: 2.48 wt% of Zn, 2.45 wt% of La, 3.91 wt% of Y, 0.32 wt% of Y, less than 0.1 wt% of the total amount of impurity elements Fe, Cu, Si and Ni, and the balance of magnesium.
And testing the high-temperature and high-pressure creep resistance of the alloy according to the standard of GB/T2039-2012 'test method for uniaxial tensile creep of metal materials'. The experimental result shows that the creep rate at 200 ℃ and 120MPa is less than 1 multiplied by 10-9/s。
From the above embodiments, the present invention provides a high temperature and high pressure creep resistant die-cast magnesium alloy, including: 1-6 wt% of Zn, 0.5-4 wt% of La, 0.5-6 wt% of Y, 0-0.5 wt% of Zr, 0-0.5 wt% of Mn, less than 0.1 wt% of impurity elements such as Si, Fe, Ni, Cu and Be, and the balance of magnesium.
The high-temperature and high-pressure resistant creep die-casting magnesium alloy contains Zn, La and Y, and the Zn, the La and the Y form second-phase grids which are formed by a plurality of crystal structures and are continuously distributed in a three-dimensional space after being melted, and the second-phase space network structures can effectively hinder dislocation slippage and twin crystal formation under a high-temperature condition, so that the resistance of alloy deformation is improved; in addition, Zn and Y in the magnesium matrix of the alloy can form basal plane precipitated phases in the creep process, thereby effectively hindering basal plane dislocation slippage; therefore, the alloy provided by the invention has extremely excellent high-temperature and high-pressure creep resistance.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make several improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the protection scope of the claims of the present invention. The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention, and many modifications of these embodiments will be apparent to those skilled in the art. The general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A high temperature and high pressure creep resistant die-cast magnesium alloy, comprising:
1-6 wt% of Zn, 0.5-4 wt% of La, 0.5-6 wt% of Y, 0-0.5 wt% of Zr, 0-0.5 wt% of Mn, and the balance of magnesium and inevitable impurity elements.
2. The die-casting magnesium alloy with high temperature and high pressure creep resistance as claimed in claim 1, wherein the mass content of Zn is 3-5%; the mass content of the La is 1.5-3%; the mass content of Y is 2.5-4.5 wt%.
3. The method for preparing the high temperature and high pressure creep resistant die casting magnesium alloy as claimed in claim 1 or 2, characterized by comprising the following steps:
1) taking a magnesium source, a zinc source, a lanthanum source, an yttrium source, a zirconium source and a manganese source according to the composition, and smelting to obtain an alloy liquid;
2) and (2) carrying out high-pressure casting on the alloy liquid obtained in the step 1) to obtain the high-temperature and high-pressure creep-resistant die-casting magnesium alloy.
4. The method for preparing the die-casting magnesium alloy with high temperature and high pressure creep resistance according to claim 3, wherein the smelting temperature in the step 1) is 700-760 ℃.
5. The preparation method of the high temperature and high pressure creep resistant die-casting magnesium alloy according to claim 3, characterized in that in the step 1), smelting is carried out under the condition of protective gas, and the protective gas is SF with a volume ratio of 1 (50-120)6And CO2。
6. The method for preparing the die-casting magnesium alloy with high temperature and high pressure creep resistance according to claim 3, wherein in the step 1), the magnesium source, the zinc source, the lanthanum source, the yttrium source, the zirconium source and the manganese source are preheated before being smelted, and the preheating temperature is 180-400 ℃.
7. The method for preparing the creep resistant die-casting magnesium alloy according to claim 3, wherein the step 1) is as follows:
1a) taking a magnesium source, a zinc source, a lanthanum source, an yttrium source, a zirconium source and a manganese source according to the composition;
1b) smelting a magnesium source, a lanthanum source and an yttrium source to obtain a first mixed molten metal;
1c) mixing a zirconium source, a manganese source and the first mixed molten metal obtained in the step 1b) to obtain a second mixed molten metal;
1d) and mixing the second mixed metal liquid with a zinc source to obtain alloy liquid.
8. The method as claimed in claim 7, wherein the mixing time of the zirconium source, the manganese source and the first mixed molten metal in step 1c) is 5-10 min, the mixing temperature is 720-750 ℃, and the mixing time of the second mixed molten metal and the zinc source in step 1d) is 8-20 min.
9. The method for preparing a high temperature and high pressure creep resistant die-cast magnesium alloy according to claim 3, wherein in the step 2), the alloy liquid is left to stand for 20min to 45min before the alloy liquid is subjected to high pressure casting, and the temperature of the alloy liquid during standing is 700 ℃ to 720 ℃.
10. The preparation method of the high-temperature and high-pressure creep resistant die-casting magnesium alloy according to claim 3, wherein the high-pressure casting in the step 2) is a cold chamber die-casting machine, and the temperature of a die-casting melt is 700-730 ℃; the preheating temperature of the die-casting die is 180-300 ℃.
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