CN103074531B - Heat resistant alloy of rare earth and magnesium and preparation method thereof - Google Patents

Heat resistant alloy of rare earth and magnesium and preparation method thereof Download PDF

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CN103074531B
CN103074531B CN201310011314.7A CN201310011314A CN103074531B CN 103074531 B CN103074531 B CN 103074531B CN 201310011314 A CN201310011314 A CN 201310011314A CN 103074531 B CN103074531 B CN 103074531B
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alloy
magnesium
rare earth
heat resisting
treatment
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CN103074531A (en
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李全安
付三玲
张清
陈君
刘文健
陈志�
宋晓杰
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Henan University of Science and Technology
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Abstract

The invention discloses a heat resistant alloy of rare earth and magnesium and a preparation method thereof. The alloy comprises the following components in percentage by weight: 6-15 percent of Gd, 0.4-1.5 percent of Sm, 0.3-1 percent of Zr, less than 0.02 percent of impurity elements including Si, Fe, Cu and Ni in total, and Mg in balancing amount. Moreover, the preparation method of the alloy is also disclosed. The heat resistant alloy of the rare earth and magnesium not only retains high-temperature tensile strength, but also is lower in cost; when the room temperature is within 250 DEG C, the tensile strength of the alloy has an anomalous temperature effect, namely the tensile strength is improved along with the raise of the temperature and is relatively reduced after the temperature reaches a certain degree; and the alloy has a broad application prospect in the field of aerospace, automobile industry, weaponry and the like.

Description

A kind of heat resisting magnesium-rare earth alloy and preparation method thereof
Technical field
The invention belongs to technical field of metal, be specifically related to a kind of heat resisting magnesium-rare earth alloy and preparation method thereof.
Background technology
Magnesium is the lightest structural metallic materials, automobile is applied increasing.The every loss of weight 100Kg of automobile, per 100 km fuel-economizing 0.5L, reduces exhaust emissions simultaneously, therefore carries out the research and development of magnesium alloy for save energy, suppression environmental pollution important in inhibiting.But its application in aerospace, military project, automobile and other industry of the not good serious obstruction of the intensity of magnesium alloy and thermotolerance, therefore improves the important topic that the intensity of magnesium alloy and thermotolerance are development magnesium alloy materials.
Existing heat resistance magnesium alloy is mainly started with from restriction dislocation motion and strengthening crystal boundary, by suitable alloying, by introducing the high second-phase of thermostability, reduce the rate of diffusion of element in magnesium matrix or improve the object that the means such as grain boundary structure state and tissue morphology realize improving magnesium alloy hot strength and high temperature creep drag.At present, in all alloying elements, rare earth (RE) improves the most effective alloying element of magnesium alloy resistance toheat, rare earth element is in the magnesium alloy except having the function of degasification, removal of impurities, raising casting fluidity, corrosion resisting property, and most of rare earth element has larger solid solubility limit in magnesium; And with temperature decline, solid solubility sharply reduces, and can obtain larger degree of supersaturation, thus in ag(e)ing process subsequently diffusion-precipitation, dystectic rare earth compound phase; The all right crystal grain thinning of rare earth element, raising room temperature strength, and be distributed in intracrystalline and crystal boundary (mainly crystal boundary) disperse, high-melting-point rare earth compound, still can pinning intracrystalline dislocation and Grain Boundary Sliding when high temperature, thus improve the hot strength of magnesium alloy, the rate of diffusion of rare earth (RE) element in magnesium matrix is comparatively slow simultaneously, and this makes Mg-RE alloy be suitable for long term operation under comparatively high temps environment.Mg-RE(is as Mg-Gd system) alloy is important refractory alloy system, has higher hot strength and excellent creep property.The Magnesium Alloys Components of long term operation under 200 ~ 250 DEG C of conditions is at present Mg-RE system alloy, the valence electron structure special due to it and significant strengthening effect in the magnesium alloy, make Mg-RE be tied to form an important alloy system into development of high strength heat resistance magnesium alloy.
In prior art, patent CN101532106B discloses a kind of heat-resistant cast rare earth magnesium alloy, component and weight percent thereof are: 7 ~ 14%Gd, 2 ~ 5%Y, 0.3 ~ 5%Sm, 0.2 ~ 0.6%Zr, impurity element S i, Fe, the total amount of Cu and Ni is less than 0.02%, surplus is Mg, this magnesium alloy has abnormal temperature effect, at comparatively high temps, there is very high tensile strength, meet aerospace device 200 ~ 250 DEG C of tensile strength all higher than the requirement of 250MPa, but its rare earth element kind used is many, content is high, there is the problem that cost is relatively high, the tensile strength that can not reach a high temperature and cost are taken into account.
Summary of the invention
The object of this invention is to provide a kind of heat resisting magnesium-rare earth alloy, while maintenance elevated temperature tensile stretches intensity, there is lower cost.
Another object of the present invention is to provide a kind of preparation method of heat resisting magnesium-rare earth alloy.
In order to realize above object, the technical solution adopted in the present invention is: a kind of heat resisting magnesium-rare earth alloy, is made up of: 6% ~ 15%Gd the component of following mass percent, 0.4% ~ 1.5%Sm, 0.3% ~ 1%Zr, impurity element S i, Fe, Cu and Ni total amount is less than 0.02%, and surplus is Mg.
The mass percent sum of described Gd and Sm is 7.5% ~ 16.5%.
This heat resisting magnesium-rare earth alloy is that raw material melting forms by magnesium and master alloy Mg-Gd, Mg-Sm, Mg-Zr.
A preparation method for heat resisting magnesium-rare earth alloy, comprises the following steps:
1) by magnesium, master alloy Mg-Gd, Mg-Sm and Mg-Zr preheating;
2) by magnesium at CO 2+ SF 6mixed gas protected lower fusing, adds master alloy Mg-Gd, Mg-Sm in 720 ~ 740 DEG C, temperature is risen to 750 ~ 780 DEG C and adds master alloy Mg-Zr;
3) after master alloy Mg-Zr melts, remove surface scum, after temperature being risen to 770 ~ 780 DEG C, keep 10min to obtain mixed solution;
4) cast after the temperature of step 3) gained mixed solution is down to 690 ~ 730 DEG C, obtain cast alloy;
5) step 4) gained cast alloy is heat-treated, obtain described heat resisting magnesium-rare earth alloy.
Preheating temperature described in step 1) is 150 ~ 220 DEG C.
When casting in step 4), casting die is preheated to 180 ~ 250 DEG C.
Thermal treatment described in step 5) carries out solution treatment and ageing treatment successively to cast alloy.
The treatment temp of described solution treatment is 490 ~ 540 DEG C, and the treatment time is 5 ~ 20 hours.
The treatment temp of described ageing treatment is 180 ~ 250 DEG C, and the treatment time is 8 ~ 20 hours.
Heat resisting magnesium-rare earth alloy component of the present invention is Mg-Gd-Sm-Zr.The present invention adopts Gd to be the first component, the maximum solid solution degree of Gd in Mg sosoloid is 20.3wt%, solid solubility when 200 DEG C in Mg sosoloid is 3.8wt%, for ensureing that alloy obtains good Precipitation strengthening and solid solution strengthening effect, the add-on of Gd is not less than 6wt%, and increase too many in order to avoid alloy density, and alloy is too brittle, therefore Gd add-on of the present invention is not higher than 15wt%.The present invention adopts Sm to be second component, and Sm can reduce the solid solubility of Gd in Mg, thus increases the Precipitation strengthening effect of Gd; The solid solubility of Sm in magnesium is changed to: 540 DEG C, 5.7wt%; 200 DEG C, 0.4wt%, in order to make solid solution strengthening effect more obviously and cost-saving to greatest extent, Sm add-on scope of the present invention is 0.4wt% ~ 1.5wt%.The present invention adopts Zr as grain-refining agent, to put forward heavy alloyed toughness and the processing performance improving alloy.
Heat resisting magnesium-rare earth alloy of the present invention, component is Mg-Gd-Sm-Zr, relative to prior art, eliminate rare earth element y, and rare earth element Sm uses lower content range, while maintenance elevated temperature tensile stretches intensity and abnormal temperature effect, rare earth element kind is few, content is low, has lower cost; Heat resisting magnesium-rare earth alloy of the present invention is in room temperature within the scope of 250 DEG C, and its tensile strength has abnormal temperature effect, and namely along with the raising of draft temperature, tensile strength also improves thereupon, and after arriving certain temperature, being generally 300 DEG C of tensile strength can decline; Heat resisting magnesium-rare earth alloy of the present invention, has broad application prospects in aerospace, automotive industry, weaponry etc.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
The raw material magnesium Mg related in the embodiment of the present invention and master alloy Mg-Gd, Mg-Sm, Mg-Zr are commercially available prod.The purity of described raw material is the Mg of 99.9%, the Mg-30.00%Gd of 99.5%, the Mg-25.11%Sm of 99.5%, 99.5% Mg-25.00%Zr.
Embodiment 1
The heat resisting magnesium-rare earth alloy of the present embodiment, is made up of the component of following mass percent: 15%Gd, 1.5%Sm, 0.5%Zr, and impurity element S i, Fe, Cu and Ni total amount is less than 0.02%, and surplus is Mg.The mass percent sum of described Gd and Sm is 16.5%.
The preparation method of the heat resisting magnesium-rare earth alloy of the present embodiment, comprises the following steps:
1) magnesium, master alloy Mg-Gd, Mg-Sm and Mg-Zr are preheating to 150 DEG C;
2) magnesium is put into the corundum crucible being preheating to 500 DEG C, at CO 2+ SF 6under mixed gas protected, high-power rapid heating fusing, after magnesium ingot fusing, adds master alloy Mg-Gd, Mg-Sm in 720 DEG C, temperature is risen to 750 DEG C and add master alloy Mg-Zr;
3) after master alloy Mg-Zr melts, remove surface scum, after temperature being risen to 780 DEG C, keep 10min to obtain mixed solution;
4) casting steel die is heated to 250 DEG C in advance, casts after step 3) gained mixeding liquid temperature is down to 690 DEG C, obtain cast alloy;
5) heat-treated by step 4) gained cast alloy: 535 DEG C of solution treatment 6h, 230 DEG C of isothermal aging process 10h, obtain described heat resisting magnesium-rare earth alloy.
Embodiment 2
The heat resisting magnesium-rare earth alloy of the present embodiment, is made up of the component of following mass percent: 6%Gd, 1.5%Sm, 1.0%Zr, and impurity element S i, Fe, Cu and Ni total amount is less than 0.02%, and surplus is Mg.The mass percent sum of described Gd and Sm is 7.5%.
The preparation method of the heat resisting magnesium-rare earth alloy of the present embodiment, comprises the following steps:
1) magnesium, master alloy Mg-Gd, Mg-Sm and Mg-Zr are preheating to 170 DEG C;
2) magnesium is put into the corundum crucible being preheating to 500 DEG C, at CO 2+ SF 6under mixed gas protected, high-power rapid heating fusing, after magnesium ingot fusing, adds master alloy Mg-Gd, Mg-Sm in 740 DEG C, temperature is risen to 770 DEG C and add master alloy Mg-Zr;
3) after master alloy Mg-Zr melts, remove surface scum, after temperature being risen to 775 DEG C, keep 10min to obtain mixed solution;
4) casting steel die is heated to 240 DEG C in advance, casts after step 3) gained mixeding liquid temperature is down to 710 DEG C, obtain cast alloy;
5) heat-treated by step 4) gained cast alloy: 540 DEG C of solution treatment 15h, 250 DEG C of isothermal aging process 8h, obtain described heat resisting magnesium-rare earth alloy.
Embodiment 3
The heat resisting magnesium-rare earth alloy of the present embodiment, is made up of the component of following mass percent: 12%Gd, 0.4%Sm, 1.0%Zr, and impurity element S i, Fe, Cu and Ni total amount is less than 0.02%, and surplus is Mg.The mass percent sum of described Gd and Sm is 12.4%.
The preparation method of the heat resisting magnesium-rare earth alloy of the present embodiment, comprises the following steps:
1) magnesium, master alloy Mg-Gd, Mg-Sm and Mg-Zr are preheating to 190 DEG C;
2) magnesium is put into the corundum crucible being preheating to 500 DEG C, at CO 2+ SF 6under mixed gas protected, high-power rapid heating fusing, after magnesium ingot fusing, adds master alloy Mg-Gd, Mg-Sm in 730 DEG C, temperature is risen to 780 DEG C and add master alloy Mg-Zr;
3) after master alloy Mg-Zr melts, remove surface scum, after temperature being risen to 780 DEG C, keep 10min to obtain mixed solution;
4) casting steel die is heated to 220 DEG C in advance, casts after step 3) gained mixeding liquid temperature is down to 730 DEG C, obtain cast alloy;
5) heat-treated by step 4) gained cast alloy: 520 DEG C of solution treatment 5h, 200 DEG C of isothermal aging process 20h, obtain described heat resisting magnesium-rare earth alloy.
Embodiment 4
The heat resisting magnesium-rare earth alloy of the present embodiment, is made up of the component of following mass percent: 10%Gd, 1.0%Sm, 0.3%Zr, and impurity element S i, Fe, Cu and Ni total amount is less than 0.02%, and surplus is Mg.The mass percent sum of described Gd and Sm is 11.0%.
The preparation method of the heat resisting magnesium-rare earth alloy of the present embodiment, comprises the following steps:
1) magnesium, master alloy Mg-Gd, Mg-Sm and Mg-Zr are preheating to 200 DEG C;
2) magnesium is put into the corundum crucible being preheating to 500 DEG C, at CO 2+ SF 6under mixed gas protected, high-power rapid heating fusing, after magnesium ingot fusing, adds master alloy Mg-Gd, Mg-Sm in 735 DEG C, temperature is risen to 760 DEG C and add master alloy Mg-Zr;
3) after master alloy Mg-Zr melts, remove surface scum, after temperature being risen to 770 DEG C, keep 10min to obtain mixed solution;
4) casting steel die is heated to 200 DEG C in advance, casts after step 3) gained mixeding liquid temperature is down to 700 DEG C, obtain cast alloy;
5) heat-treated by step 4) gained cast alloy: 500 DEG C of solution treatment 20h, 180 DEG C of isothermal aging process 15h, obtain described heat resisting magnesium-rare earth alloy.
Embodiment 5
The heat resisting magnesium-rare earth alloy of the present embodiment, is made up of the component of following mass percent: 15%Gd, 1.5%Sm, 0.8%Zr, and impurity element S i, Fe, Cu and Ni total amount is less than 0.02%, and surplus is Mg.The mass percent sum of described Gd and Sm is 16.5%.
The preparation method of the heat resisting magnesium-rare earth alloy of the present embodiment, comprises the following steps:
1) magnesium, master alloy Mg-Gd, Mg-Sm and Mg-Zr are preheating to 220 DEG C;
2) magnesium is put into the corundum crucible being preheating to 500 DEG C, at CO 2+ SF 6under mixed gas protected, high-power rapid heating fusing, after magnesium ingot fusing, adds master alloy Mg-Gd, Mg-Sm in 725 DEG C, temperature is risen to 765 DEG C and add master alloy Mg-Zr;
3) after master alloy Mg-Zr melts, remove surface scum, after temperature being risen to 770 DEG C, keep 10min to obtain mixed solution;
4) casting steel die is heated to 180 DEG C in advance, casts after step 3) gained mixeding liquid temperature is down to 720 DEG C, obtain cast alloy;
5) heat-treated by step 4) gained cast alloy: 490 DEG C of solution treatment 10h, 240 DEG C of isothermal aging process 18h, obtain described heat resisting magnesium-rare earth alloy.
Experimental example
This experimental example carries out tensile strength experiment to embodiment 1 ~ 5 gained heat resisting magnesium-rare earth alloy, experimental technique is: by the sample of gained heat resisting magnesium-rare earth alloy, be processed into 5 times of standard tensile specimen according to standard GB/T 6397-86 " metal stretching experimental sample ", tension specimen at high temperature needs in sample two ends machining screw to meet the requirement of the clamping device of drawing by high temperature sample.Electronics is stretching on the accurate universal testing machine of Japanese Shimadzu AG-I250kN and carries out, and draw speed is 1mm/min; During drawing by high temperature, at the corresponding temperature to tension specimen insulation 15min, temperature fluctuation ± 1 DEG C, then stretches.Experimental result is as shown in table 1:
The tensile strength experimental result of table 1 embodiment 1 ~ 5 gained heat resisting magnesium-rare earth alloy
As can be seen from Table 1, the heat resisting magnesium-rare earth alloy of embodiment 1 ~ 5, component is Mg-Gd-Sm-Zr, relative to comparative example 1 ~ 3, eliminate rare earth element y, and rare earth element Sm uses lower content range, while maintenance elevated temperature tensile stretches intensity and abnormal temperature effect, rare earth element kind is few, and content is low, has lower cost.

Claims (9)

1. a heat resisting magnesium-rare earth alloy, is characterized in that: be made up of the component of following mass percent: 6% ~ 15%Gd, 0.4% ~ 1.5%Sm, 0.3% ~ 1%Zr, and impurity element S i, Fe, Cu and Ni total amount is less than 0.02%, and surplus is Mg; Its preparation method comprises the following steps:
1) by magnesium, master alloy Mg-Gd, Mg-Sm and Mg-Zr preheating;
2) by magnesium at CO 2+ SF 6mixed gas protected lower fusing, adds master alloy Mg-Gd, Mg-Sm in 720 ~ 740 DEG C, temperature is risen to 750 ~ 780 DEG C and adds master alloy Mg-Zr;
3) after master alloy Mg-Zr melts, remove surface scum, after temperature being risen to 770 ~ 780 DEG C, keep 10min to obtain mixed solution;
4) until step 3) temperature of gained mixed solution casts after being down to 690 ~ 730 DEG C, obtains cast alloy;
5) by step 4) gained cast alloy heat-treats, and obtains described heat resisting magnesium-rare earth alloy;
Wherein step 5) described in thermal treatment be that successively solution treatment and ageing treatment are carried out to cast alloy, the treatment temp of solution treatment is 490 ~ 540 DEG C, treatment time is 5 ~ 20 hours, and the treatment temp of ageing treatment is 180 ~ 250 DEG C, and the treatment time is 8 ~ 20 hours.
2. heat resisting magnesium-rare earth alloy according to claim 1, is characterized in that: the mass percent sum of described Gd and Sm is 7.5% ~ 16.5%.
3. heat resisting magnesium-rare earth alloy according to claim 1, is characterized in that: this heat resisting magnesium-rare earth alloy is that raw material melting forms by magnesium and master alloy Mg-Gd, Mg-Sm, Mg-Zr.
4. a preparation method for heat resisting magnesium-rare earth alloy as claimed in claim 1, is characterized in that: comprise the following steps:
1) by magnesium, master alloy Mg-Gd, Mg-Sm and Mg-Zr preheating;
2) by magnesium at CO 2+ SF 6mixed gas protected lower fusing, adds master alloy Mg-Gd, Mg-Sm in 720 ~ 740 DEG C, temperature is risen to 750 ~ 780 DEG C and adds master alloy Mg-Zr;
3) after master alloy Mg-Zr melts, remove surface scum, after temperature being risen to 770 ~ 780 DEG C, keep 10min to obtain mixed solution;
4) until step 3) temperature of gained mixed solution casts after being down to 690 ~ 730 DEG C, obtains cast alloy;
5) by step 4) gained cast alloy heat-treats, and obtains described heat resisting magnesium-rare earth alloy.
5. the preparation method of heat resisting magnesium-rare earth alloy according to claim 4, is characterized in that: step 1) described in preheating temperature be 150 ~ 220 DEG C.
6. the preparation method of heat resisting magnesium-rare earth alloy according to claim 4, is characterized in that: step 4) in casting time casting die is preheated to 180 ~ 250 DEG C.
7. the preparation method of heat resisting magnesium-rare earth alloy according to claim 4, is characterized in that: step 5) described in thermal treatment be that successively solution treatment and ageing treatment are carried out to cast alloy.
8. the preparation method of heat resisting magnesium-rare earth alloy according to claim 7, is characterized in that: the treatment temp of described solution treatment is 490 ~ 540 DEG C, and the treatment time is 5 ~ 20 hours.
9. the preparation method of heat resisting magnesium-rare earth alloy according to claim 7, is characterized in that: the treatment temp of described ageing treatment is 180 ~ 250 DEG C, and the treatment time is 8 ~ 20 hours.
CN201310011314.7A 2013-01-11 2013-01-11 Heat resistant alloy of rare earth and magnesium and preparation method thereof Expired - Fee Related CN103074531B (en)

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CN103421999B (en) * 2013-07-15 2016-01-20 中南大学 A kind of containing Heat Resistant Rare Earth-magnesium Alloy and preparation method thereof
CN108300920B (en) * 2018-02-09 2019-08-09 河南科技大学 A kind of high-strength anti-flaming magnesium alloy and preparation method thereof
CN109321795B (en) * 2018-11-01 2020-10-30 贵州航天风华精密设备有限公司 Magnesium alloy with electromagnetic shielding performance
CN109468513A (en) * 2018-12-18 2019-03-15 上海交通大学 A kind of high-strength temperature-resistant casting magnesium-rare earth alloy and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN101008060A (en) * 2006-11-30 2007-08-01 中国科学院长春应用化学研究所 Heat-proof magnesium-base rare earth alloy and its preparation method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101008060A (en) * 2006-11-30 2007-08-01 中国科学院长春应用化学研究所 Heat-proof magnesium-base rare earth alloy and its preparation method

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