CN103421999B - A kind of containing Heat Resistant Rare Earth-magnesium Alloy and preparation method thereof - Google Patents
A kind of containing Heat Resistant Rare Earth-magnesium Alloy and preparation method thereof Download PDFInfo
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Abstract
The present invention's one, containing Heat Resistant Rare Earth-magnesium Alloy and preparation method thereof, belongs to technical field of magnesium alloy preparation.Of the present invention containing Heat Resistant Rare Earth-magnesium Alloy, its component comprises by percentage to the quality: Sm2%-8%, Gd0.5%-6%, Zn0.1%-2%, Zr0.1%-1.5%, all the other are Mg and inevitable impurity element; Impurity element total amount≤0.02%.The present invention replaces Y, Nd in WE series alloy by interpolation alloying element (Sm, Gd, Zn), and adjusts corresponding thermal treatment process, makes prepared magnesium alloy have excellent room temperature strength, hot strength and plasticity; Magnesium alloy prepared by the present invention has the mechanical properties such as more superior room temperature strength, hot strength than traditional WE series business magnesium alloy, and its preparation cost is also lower than the preparation cost of WE series business magnesium alloy.Present invention process is simple, is convenient to commercial application.
Description
Technical field
The present invention relates to a kind of heat resistance magnesium alloy and preparation method thereof, be specifically related to a kind of low cost and contain heat resistance magnesium alloy of rare earth zincification and preparation method thereof.
Background technology
The not good paces hindering magnesium alloy and replace the materials such as aluminium alloy in aerospace, military project and other industry of undercapacity and thermotolerance.Rare earth element, owing to having unique configuration of extra-nuclear electron, shows unique character, can purify alloy melt, improves alloy structure in metallurgical process, improves Alloy At Room Temperature and mechanical behavior under high temperature and enhancing alloy corrosion resistance.WE43 alloy (3.7 ~ 4.3%Y, 2.4 ~ 4.4%Nd, 0.4%Zr, surplus Mg) its use temperature under the prerequisite of guaranteed performance can reach 200 DEG C, and after T6 process, room temperature tensile intensity is 250MPa, and yield strength is 178MPa, and unit elongation is 7.0%; Tensile strength at 200 DEG C and unit elongation are 211MPa and 11%.But in its castingprocesses, molten state is oxidizable and produce L&S line defect, causes casting technique harsher and increases cost.Its deficiency of above-mentioned alloy is, lower room-temperature mechanical property limits the widespread use of WE43 alloy.WE43 alloy, after T6 process, separates out β ' and thick β in matrix
1phase, is shown in accompanying drawing 1, due to β
1the appearance of phase causes the mechanical property of alloy to reduce.
Summary of the invention
The object of the invention is to overcome deficiency of the prior art, propose a kind ofly to have heat resistance magnesium alloy that intensity is high and plasticity is good and preparation method thereof concurrently, Y, the Nd in WE series alloy is replaced by interpolation alloying element (Sm, Gd, Zn), and adjust corresponding thermal treatment process, achieving heat resistance magnesium alloy needs the room temperature strength of the excellence possessed, hot strength and plasticity to make this type of magnesium alloy have mechanical property and the lower cost of alloy such as room temperature strength, hot strength more superior than traditional WE series business magnesium alloy.
One of the present invention is containing Heat Resistant Rare Earth-magnesium Alloy, and its component comprises by percentage to the quality:
Sm2%-8%；
Gd0.5%-6%；
Zn0.1%-2%；
Zr0.1%-1.5%；
All the other are Mg and inevitable impurity element; Ratio≤0.02% of impurity element total mass and alloy total mass.
One of the present invention is containing Heat Resistant Rare Earth-magnesium Alloy, and its component comprises by percentage to the quality:
Sm3%-6%；
Gd2%-5%；
Zn0.1%-2%；
Zr0.1%-1.5%；
All the other are Mg and inevitable impurity element; Ratio≤0.02% of impurity element total mass and alloy total mass; Impurity element comprises Fe, Cu, Ni; The wherein quality of Fe and ratio≤0.005% of alloy total mass, the quality of Cu and ratio≤0.01% of alloy total mass, the quality of Ni and ratio≤0.001% of alloy total mass.The corrosion resisting property of alloy significantly reduces along with the increase of magazine content.
A kind of preparation method containing Heat Resistant Rare Earth-magnesium Alloy of the present invention, comprises the steps:
Step one is prepared burden
Join by the alloy compositions proportioning of design and get magnesium ingot, zinc ingot metal, Mg-Sm master alloy, Mg-Gd master alloy, Mg-Zr master alloy as starting material;
Step 2 founding
Under a shielding gas, magnesium ingot is added heat fused in smelting furnace, be warming up to 680 ~ 720 DEG C and add zinc ingot metal; after stirring fusing, be warming up to 720 ~ 740 DEG C, in magnesium liquid, add Mg-Sm and Mg-Gd master alloy successively; be warming up to 760 ~ 780 DEG C of insulations after fusing, add Mg-Zr master alloy, after fusing; be warming up to 780 ~ 800 DEG C, after samming, be cooled to 740 ~ 760 DEG C; carry out insulation refining; then, leave standstill and be cooled to 700 ~ 740 DEG C and cast, obtain magnesium-rare earth alloy ingot casting base.
A kind of preparation method containing Heat Resistant Rare Earth-magnesium Alloy of the present invention, the starting material of each component of alloy in air furnace dry 2 ~ 4 hours, described drying temperature is 180 ~ 220 DEG C.
A kind of preparation method containing Heat Resistant Rare Earth-magnesium Alloy of the present invention, smelting furnace is electrical crucible.
A kind of preparation method containing Heat Resistant Rare Earth-magnesium Alloy of the present invention, when magnesium liquid temp reaches 680 ~ 720 DEG C, adds zinc ingot metal, stirs fusing.
A kind of preparation method containing Heat Resistant Rare Earth-magnesium Alloy of the present invention, purity >=99.99% of magnesium ingot, purity >=99.99% of zinc ingot metal, the foreign matter content of Mg-Sm, Mg-Gd and Mg-Zr master alloy is not higher than 0.1%.
A kind of preparation method containing Heat Resistant Rare Earth-magnesium Alloy of the present invention, after Mg-Zr master alloy adds, is 15 ~ 30min in the time of 780 ~ 800 DEG C of sammings; Refining temperature is 740 ~ 760 DEG C, and refining time is 5 ~ 10min.
A kind of preparation method containing Heat Resistant Rare Earth-magnesium Alloy of the present invention, the standing time is 15 ~ 30min.
A kind of preparation method containing Heat Resistant Rare Earth-magnesium Alloy of the present invention, shielding gas described in step 2 is SF
6and CO
2mixed gas; Its volume ratio is 1:90-105, and the flow of shielding gas is 10mL/s.
A kind of preparation method containing Heat Resistant Rare Earth-magnesium Alloy of the present invention, magnesium-rare earth alloy ingot blank is placed in 70 ~ 80 DEG C of hot water immediately and quenches after 480 ~ 550 DEG C of insulation 4 ~ 24h carry out solution treatment, in air furnace, be incubated 8 ~ 36h again, aging temperature is 175 ~ 250 DEG C.
Principle and advantage
At eutectic temperature, rare earth Gd and the Sm maximum solid solution degree in magnesium is 23.3wt.% and 5.8wt.%, be greater than the 3.6wt.% of 12.0wt.% and Nd of Y respectively, and its solid solubility significantly declines along with the reduction of temperature, therefore Mg-Gd, Mg-Sm binary alloy is heat-treatable strengthened magnesium alloy, the solution strengthening better than Y, Nd and ageing strengthening effect may be produced respectively, obtain better comprehensive mechanical property.The present invention is using Mg, Sm as basal component, after adding Zn element, the rich Zn rare earth compound pinning crystal boundary of generation can be utilized on the one hand, bear part load and improve high-temperature behavior, but also the aging response speed can accelerating alloy is β ' the phase that alloy substrate separates out more Dispersed precipitate, sees accompanying drawing 2.Because β ' and Mg matrix have semicoherent interface, so at high temperature contribute to suppressing matrix distortion, thus improve the thermotolerance of alloy.Add Gd element, be solid-solution in magnesium matrix, improve the effect of Sm element solid solution and ageing strengthening, adding Zr is in order to refining alloy crystal grain, improves the mechanical property of alloy further, thus can obtain comparatively excellent over-all properties.
In a word, compared with prior art, the present invention has that technique is simple, composition is reasonable, and prepared has excellent mechanical property containing Heat Resistant Rare Earth-magnesium Alloy.Because the density (7.54g/cm of Sm
3) than Gd (7.89g/cm
3) little, the Mg-Gd-Y system (addition about 10% of Gd) of addition also than general is low, so cost of alloy of the present invention is cheaper and have good plasticity and the hot strength of excellence.For Mg-4Sm-4Gd-0.5Zn-0.5Zr(weight percent), under as cast condition, its tensile strength and unit elongation are respectively 238.6MPa and 5.3%, alloy founding obtained carries out 530 DEG C, after the solution treatment (being called for short T4) of 16h, room temperature tensile intensity and unit elongation are respectively 256.7MPa and 8.5%, 225 DEG C are carried out again after above-mentioned solution treatment, the ageing treatment of 24h, room temperature tensile intensity and unit elongation are respectively 310.4MPa and 4.8%, improve 60.4Mpa relative to the room temperature tensile intensity of WE43 alloy after T6 process; The tensile strength of its high temperature 200 DEG C, up to 278MPa, improves 67Mpa relative to the tensile strength of the high temperature 200 DEG C of WE43 alloy after T6 process.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of existing WE43 alloy after T6 process;
The transmission electron microscope picture of the magnesium-rare earth alloy of Fig. 2 prepared by example 2 after T6 process;
In Fig. 1,1 is thick β 1 phase, and 2 is tiny β ' phase; WE43 alloy is after T6 process as can be seen from Figure 1, separates out β ' and thick β 1 phase in matrix.
In Fig. 2,2 is tiny β ' phase; Magnesium-rare earth alloy as can be seen from Figure 2 prepared by embodiment 2 alloy substrate after T6 process separate out β ' be uniformly distributed in disperse mutually.
Embodiment
Below embodiments of the invention are elaborated: the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
The foreign matter content of purity >=99.99% of the magnesium ingot adopted in embodiment, purity >=99.99% of zinc ingot metal, Mg-Sm, Mg-Gd and Mg-Zr master alloy is not all higher than 0.1wt%.
Embodiment 1:
Alloying constituent (weight percent): 3%Sm, 2%Gd, 0.5%Zn, 0.5%Zr, impurity element is less than 0.02%, and all the other are Mg.
The melting technology of this alloy is: according to mentioned component alloyage, and in the baking oven of 180 DEG C, raw material is fully dry, adds pure magnesium, adopt SF simultaneously in electrical crucible
6and CO
2mixed gas (1:95) protect, after magnesium ingot melts completely, at 680 DEG C, add industrial-purity zinc, stir fusing after; When adding Mg-Sm master alloy after magnesium liquid temp reaches 720 DEG C in magnesium liquid, when magnesium liquid temp goes back up to 720 DEG C after Mg-Sm fusing, add Mg-Gd master alloy again; Add Mg-Zr master alloy after magnesium liquid temp is risen to 780 DEG C, stir 2min and make it fully melt; Be warming up to 790 DEG C and be cooled to 760 DEG C after being incubated 15min, refining 5min, leaving standstill after refining, time of repose controls between 30min, after magnesium liquid is cooled to 730 DEG C, skim surface scum cast, casting steel die is heated to 200 DEG C in advance, namely obtains magnesium-rare earth alloy ingot blank.
Alloy founding obtained carries out 530 DEG C, after the solution treatment of 4h (being called for short T4) or T4 process, is placed in 80 DEG C of hot water immediately and quenches, then carry out 200 DEG C, the ageing treatment (abbreviation T6) of 24h.Finally can obtain the heat-resisting Mg-3Sm-2Gd-0.5Zn-0.5Zr alloy having high strength and good plasticity concurrently.
The alloy of the present embodiment, under as cast condition, its room temperature tensile intensity and unit elongation are respectively 212.9MPa and 6.7%, and after T4 process, room temperature tensile intensity and unit elongation are respectively 227MPa and 10.6%, after T6 process, room temperature tensile intensity and unit elongation are respectively 268.1MPa and 8.9%; Improve 18.1Mpa relative to the room temperature tensile intensity of WE43 alloy after T6 process, unit elongation also has obvious lifting.
The alloy of the present embodiment, after T6 process, the tensile strength of high temperature 200 DEG C test is 225MPa; 14Mpa is improve relative to the tensile strength of the high temperature 200 DEG C of WE43 alloy after T6 process.
Embodiment 2:
Alloying constituent (weight percent): 4%Sm, 4%Gd, 0.5%Zn, 0.5%Zr, impurity element is less than 0.02%, and all the other are Mg.
The melting technology of this alloy is: according to mentioned component alloyage, and in the baking oven of 200 DEG C, raw material is fully dry, adds pure magnesium, adopt SF simultaneously in electrical crucible
6and CO
2mixed gas (1:100) protect, after magnesium ingot melts completely, at 700 DEG C, add industrial-purity zinc, stir fusing after; When adding Mg-Sm master alloy after magnesium liquid temp reaches 720 DEG C in magnesium liquid, when magnesium liquid temp goes back up to 720 DEG C after Mg-Sm fusing, add Mg-Gd master alloy again; Add Mg-Zr master alloy after magnesium liquid temp is risen to 760 DEG C, stir 2min and make it fully melt; Be warming up to 800 DEG C and be cooled to 740 DEG C after being incubated 20min, refining 10min, leaving standstill after refining, time of repose controls between 30min, after magnesium liquid is cooled to 700 DEG C, skim surface scum cast, casting steel die is heated to 200 DEG C in advance, namely obtains magnesium-rare earth alloy ingot blank.
Alloy founding obtained carries out 550 DEG C, after the solution treatment of 16h (being called for short T4) or T4 process, is placed in 75 DEG C of hot water immediately and quenches, then carry out 225 DEG C, the ageing treatment (abbreviation T6) of 24h.Finally can obtain the heat-resisting Mg-4Sm-4Gd-0.5Zn-0.5Zr alloy having high strength and good plasticity concurrently, its transmission electron microscope picture is shown in Fig. 2.
The alloy of the present embodiment, under as cast condition, its room temperature tensile intensity and unit elongation are respectively 238.6MPa and 5.3%, and after T4 process, room temperature tensile intensity and unit elongation are respectively 256.7MPa and 8.5%, after T6 process, room temperature tensile intensity and unit elongation are respectively 310.4MPa and 4.8%; 60.4Mpa is improve relative to the room temperature tensile intensity of WE43 alloy after T6 process.
The alloy of the present embodiment, after T6 process, the tensile strength of high temperature 200 DEG C test is up to 278MPa; 67Mpa is improve relative to the tensile strength of the high temperature 200 DEG C of WE43 alloy after T6 process.
Example 3:
Alloying constituent (weight percent): 5%Sm, 5%Gd, 1%Zn, 0.5%Zr, impurity element is less than 0.02%, and all the other are Mg.
The melting technology of this alloy is: according to mentioned component alloyage, and in the baking oven of 220 DEG C, raw material is fully dry, adds pure magnesium, adopt SF simultaneously in electrical crucible
6and CO
2mixed gas (1:105) protect, after magnesium ingot melts completely, at 720 DEG C, add industrial-purity zinc; When adding Mg-Sm master alloy after magnesium liquid temp reaches 740 DEG C in magnesium liquid, when magnesium liquid temp goes back up to 740 DEG C after Mg-Sm fusing, add Mg-Gd master alloy again; Add Mg-Zr master alloy after magnesium liquid temp is risen to 780 DEG C, stir 2min and make it fully melt; After 780 DEG C of insulation 30min, be cooled to 750 DEG C, refining 5min, leave standstill after refining, time of repose controls between 30min, after magnesium liquid is cooled to 740 DEG C, skim surface scum cast, casting steel die is heated to 200 DEG C in advance, namely obtains magnesium-rare earth alloy ingot blank.
Alloy founding obtained carries out 480 DEG C, after the solution treatment of 24h (being called for short T4) or T4 process, is placed in 70 DEG C of hot water immediately and quenches, then carry out 250 DEG C, the ageing treatment (abbreviation T6) of 36h.Finally can obtain the heat-resisting Mg-5Sm-5Gd-1Zn-0.5Zr alloy having high strength and good plasticity concurrently.
The alloy of the present embodiment, under as cast condition, its room temperature tensile intensity and unit elongation are respectively 253MPa and 6%, and after T4 process, room temperature tensile intensity and unit elongation are respectively 260MPa and 9%, and after T6 process, room temperature tensile intensity and unit elongation are respectively 301MPa and 3.3%; 51Mpa is improve relative to the room temperature tensile intensity of WE43 alloy after T6 process.
The alloy of the present embodiment, after T6 process, the tensile strength of high temperature 200 DEG C test is up to 268MPa; 57Mpa is improve relative to the tensile strength of the high temperature 200 DEG C of WE43 alloy after T6 process.
Can find out that from above-mentioned example the principal element samarium of heat resistance magnesium alloy of the present invention and gadolinium are the absolute factors that the present invention has high-strength temperature-resistant performance at 2 ~ 8% and 0.5 ~ 6% weight ratio respectively, when the weight of samarium and gadolinium accounts for 5 ~ 8% of gross weight of the present invention, the present invention has good mechanical property and cost advantages.
It should be noted last that, above example is only illustrative rather than definitive thereof technical scheme of the present invention, although with reference to above-described embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: still can modify to the present invention or equivalent replacement, and not departing from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (7)
1., containing a Heat Resistant Rare Earth-magnesium Alloy, its component comprises by percentage to the quality:
Sm3％-6％；
Gd2％-5％；
Zn0.1％-2％；
Zr0.1％-1.5％；
All the other are Mg and inevitable impurity element; Impurity element total amount≤0.02%;
The described preparation method containing Heat Resistant Rare Earth-magnesium Alloy, comprises the steps:
Step one is prepared burden
Join by the alloy compositions proportioning of design and get magnesium ingot, zinc ingot metal, Mg-Sm master alloy, Mg-Gd master alloy, Mg-Zr master alloy as starting material;
Step 2 founding
Under a shielding gas, magnesium ingot is added heat fused in smelting furnace, be warming up to 680 ~ 720 DEG C and add zinc ingot metal, after stirring fusing, be warming up to 720 ~ 740 DEG C, in magnesium liquid, add Mg-Sm and Mg-Gd master alloy successively, be warming up to 760 ~ 780 DEG C of insulations after fusing, add Mg-Zr master alloy, after fusing, be warming up to 780 ~ 800 DEG C, after samming, be cooled to 740 ~ 760 DEG C, carry out insulation refining, then, leave standstill and be cooled to 700 ~ 740 DEG C and cast, obtain magnesium-rare earth alloy ingot casting base;
Magnesium-rare earth alloy ingot casting base is placed in 70 ~ 80 DEG C of hot water immediately and quenches after 480 ~ 550 DEG C of insulation 4 ~ 24h carry out solution treatment, then is incubated 8 ~ 36h in air furnace, and carry out ageing treatment, during ageing treatment, control temperature is 175 ~ 250 DEG C.
2. one according to claim 1 is containing Heat Resistant Rare Earth-magnesium Alloy; It is characterized in that: the starting material of each component of alloy in air furnace dry 2 ~ 4 hours, drying temperature is 180 ~ 220 DEG C.
3. one according to claim 1 is containing Heat Resistant Rare Earth-magnesium Alloy, it is characterized in that: smelting furnace is electrical crucible.
4. one according to claim 1 is containing Heat Resistant Rare Earth-magnesium Alloy, and it is characterized in that: purity >=99.99% of magnesium ingot, purity >=99.99% of zinc ingot metal, the foreign matter content of Mg-Sm, Mg-Gd and Mg-Zr master alloy is not higher than 0.1%.
5. one according to claim 1 is containing Heat Resistant Rare Earth-magnesium Alloy, it is characterized in that: equal temperature time is 15 ~ 30min; The time of insulation refining is 5 ~ 10min.
6. one according to claim 1 is containing Heat Resistant Rare Earth-magnesium Alloy, it is characterized in that: the time left standstill is 15 ~ 30min.
7. one according to claim 1 is containing Heat Resistant Rare Earth-magnesium Alloy, it is characterized in that: shielding gas described in step 2 is SF
6and CO
2mixed gas; SF
6with CO
2volume ratio be 1:95-105.
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| CN104946949B (en) * | 2015-06-17 | 2017-02-22 | 西安建筑科技大学 | Novel yttrium samarium magnesium alloy and preparation method thereof |
| CN105463282A (en) * | 2015-12-03 | 2016-04-06 | 嘉瑞科技（惠州）有限公司 | Rare earth-magnesium alloy and preparation method thereof |
| CN107739938B (en) * | 2017-10-24 | 2019-05-14 | 重庆理工大学 | A kind of Mg-Sr-Mn system heat resistance magnesium alloy and preparation method thereof |
| CN107904465B (en) * | 2017-11-20 | 2019-09-20 | 河南科技大学 | A kind of enhancing magnesium-based composite material and preparation method thereof |
| CN108754267A (en) * | 2018-06-12 | 2018-11-06 | 中国科学院长春应用化学研究所 | High-strength deforming magnesium alloy and preparation method thereof containing rare earth samarium |
| CN108796328B (en) * | 2018-07-03 | 2020-05-19 | 中国科学院长春应用化学研究所 | High-strength heat-resistant rare earth magnesium alloy and preparation method thereof |
| CN109022984B (en) * | 2018-09-25 | 2021-01-19 | 中国科学院海洋研究所 | Zn-containing corrosion-resistant rare earth magnesium alloy and preparation method thereof |
| CN109811162B (en) * | 2019-04-03 | 2020-06-26 | 河南科技大学 | Antimony-containing rare earth magnesium alloy and preparation method thereof |
| CN114351020B (en) * | 2021-12-30 | 2022-12-13 | 台山市中镁科技有限公司 | Magnesium alloy casting and preparation method and application thereof |
| CN114525421B (en) * | 2022-01-25 | 2023-03-14 | 台山市中镁科技有限公司 | Magnesium alloy and preparation method and application thereof |
| CN114686711B (en) * | 2022-03-11 | 2023-06-23 | 上海交通大学 | High-strength and high-toughness cast magnesium rare earth alloy capable of being subjected to rapid high-temperature solution treatment and preparation method thereof |
| CN114807706B (en) * | 2022-05-16 | 2023-07-14 | 洛阳理工学院 | High-performance wrought magnesium alloy and preparation method thereof |
| CN114850727B (en) * | 2022-05-19 | 2023-01-20 | 吉林大学 | High-performance antioxidant rare earth magnesium alloy ultra-long thin wire and preparation method thereof |
| CN114921701B (en) * | 2022-05-24 | 2023-06-02 | 洛阳理工学院 | Rare earth magnesium alloy and preparation method thereof |
| CN115896513A (en) * | 2022-12-26 | 2023-04-04 | 西安四方超轻材料有限公司 | Rare earth adding method for rare earth-containing magnesium alloy |
| CN117660819B (en) * | 2024-01-25 | 2024-05-07 | 龙南龙钇重稀土科技股份有限公司 | Gao Jiangke magnesium-dissolving alloy and preparation method thereof |
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| CN101503774A (en) * | 2009-03-09 | 2009-08-12 | 西北工业大学 | Casting magnesium alloy material and preparation thereof |
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