CN100457945C - Wrought magnesium alloys in high intensity, high plasticity, and preparation method - Google Patents
Wrought magnesium alloys in high intensity, high plasticity, and preparation method Download PDFInfo
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- CN100457945C CN100457945C CNB2007100222168A CN200710022216A CN100457945C CN 100457945 C CN100457945 C CN 100457945C CN B2007100222168 A CNB2007100222168 A CN B2007100222168A CN 200710022216 A CN200710022216 A CN 200710022216A CN 100457945 C CN100457945 C CN 100457945C
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- earth element
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 28
- 239000000956 alloy Substances 0.000 claims abstract description 28
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 24
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 17
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 15
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000011777 magnesium Substances 0.000 claims description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 17
- 238000007670 refining Methods 0.000 claims description 17
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 230000004907 flux Effects 0.000 claims description 9
- 239000011701 zinc Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 2
- 238000010309 melting process Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 6
- 229910001093 Zr alloy Inorganic materials 0.000 abstract description 2
- 235000012438 extruded product Nutrition 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract 1
- 229910052759 nickel Inorganic materials 0.000 abstract 1
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 7
- 239000010936 titanium Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 208000035126 Facies Diseases 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- UQCVYEFSQYEJOJ-UHFFFAOYSA-N [Mg].[Zn].[Zr] Chemical compound [Mg].[Zn].[Zr] UQCVYEFSQYEJOJ-UHFFFAOYSA-N 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000001192 hot extrusion Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000029052 metamorphosis Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Abstract
This invention discloses a method for preparing Mg alloy with high strength and high plastic deformation. The compositions of the Mg alloy are: Zn 4.5-5.5 wt.%, Ce 0.5-2.5 wt.%, Ti 0.01-0.20 wt.%, Si less than or equal to 0.08 wt.%, Fe less than or equal to 0.01 wt.%, Cu less than or equal to 0.01 wt.%, Ni less than or equal to 0.002 wt.%, impurities less than or equal to 0.05 wt.%, and Mg as balance. The method adds rare earth element Ce to Mg-Zn-Zr alloy, and replaces Zr with Ti, thus can refine the alloy grains. Besides, Mg forms a dispersed reinforcing phase, which can effectively improve the comprehensive properties of the Mg alloy. The surface quality of the extruded product of the Mg alloy is obviously improved when compared with ZK series deformed Mg alloys. The average tensile strength, yield strength and elongation at breakage of the Mg alloy at room temperature are 360 MPa, 245 MPa and 7%, respectively. The average tensile strength and elongation at breakage of the Mg alloy at 150 deg.C are 250 MPa and 11%, respectively.
Description
Technical field
The invention belongs to the magnesium alloy production technical field, relate in particular to a kind of wrought magnesium alloys of high-strength high-plasticity.
Background technology
At present, the relatively poor plasticity of magnesium-zinc-zirconium alloy (as the ZK60 magnesium alloy) high-strength deformation material makes the hot extrusion technique condition be difficult to control.Texturing temperature is too low, can not fully start all slip systems of magnesium matrix, and alloy second to hinder metamorphosis mutually obvious, " squeezing motionless " phenomenon appears.Because the fusing point of zinc is low, can find that in alloy structure the eutectic composition segregation is more serious between dendritic arm, so the too high alloy that then makes of texturing temperature is easy to generate and burning overheated when hot-work, the squeeze wood surface quality is poor.With existing ZK60 magnesium alloy is that (moiety and weight percent content thereof are Zn:4.8～6.2%, Zr to example: other impurity elements 〉=0.45% :≤0.30%, surplus is a magnesium), it is room temperature average tensile strength 286MPa under the extruding attitude, yield strength 205MPa, elongation after fracture 5.6%, its tensile strength under 150 ℃ only are 170Mpa.
Summary of the invention
It is exactly the problem that above-mentioned ZK60 magnesium alloy exists that the present invention will solve, and a kind of wrought magnesium alloys of high-strength high-plasticity is provided.
The weight percent of each component of the present invention is: Zn:4.5～5.5%, Ce:0.5～2.5%, Ti:0.01～0.20%, Si: Fe≤0.08%: Cu≤0.01%: Ni≤0.01%: other impurity elements≤0.002% :≤0.05%, and surplus is Mg.
The preparation method that the present invention adopts may further comprise the steps:
1, adds end flux melts with dropping in the off-the-shelf clean crucible after industrial magnesium ingot, the zinc ingot metal pre-treatment, the consumption of end flux accounts for 1.5～2.5% of quality of furnace charge, be sprinkled into insulating covering agent simultaneously, the consumption of insulating covering agent accounts for 0.3～0.5% of quality of furnace charge, the whole melting process time is controlled at 2～6h, and magnesium liquid outlet temperature is controlled at 670～690 ℃;
2, after fusing finishes, be warming up to 780～810 ℃, add potassium fluotitanate and rare-earth element cerium in batches and lentamente, all after the fusing, drag for the end and stir 3～5min, make the alloy homogenizing, wherein rare-earth element cerium is preheated to 300～400 ℃;
3, the alloy liquid temp is adjusted to 750～760 ℃ of blowing argon gas refining 6～10min, adds refining agent simultaneously, the consumption of refining agent accounts for 1.5～2.5% of quality of furnace charge;
4, alloy liquid is warming up to 780～810 ℃ and leaves standstill 10～20min;
5, reduce under 690～710 ℃ of temperature condition, and pour into a mould under protective atmosphere, protective atmosphere is generally SF
6, CO
2, SO
2, dry air mixed gas or mixed gas protected atmosphere.
End flux, insulating covering agent, refining agent that the present invention adopts must be selected for use and contain or do not contain MgCl less
2Flux.
The present invention is by adding metal titanium and rare-earth element cerium, and its effect is main to show in the following areas:
1) adds metal titanium, avoid using metal zirconium to produce accumulative facies, thereby eliminate the blackout phenomenon on extruded product surface, so that obtain the surface of comparison light;
2) add rare-earth element cerium, its crystal grain inside almost all be magnesium, and zinc and cerium accumulate on the crystal boundary with the form of compound, effective crystal grain thinning, thereby raising tensile strength of alloys and elongation;
3) add rare-earth element cerium, the heat-resisting Mg mutually of cerium and magnesium formation
12Ce can hinder recrystal grain and grow up, thereby obtains tiny dynamic recrystallization crystal grain after the extruding, all is useful for improving tensile strength of alloys and elongation;
4) add rare-earth element cerium, the precipitated phase particle that contains Ce and Zn in the alloy extrusion process is banded disperse along the direction of extrusion and distributes after fragmentation, thus the intensity that effectively the improves alloy surface quality of finished product particularly;
5) add rare-earth element cerium, alloy fracture a large amount of dimples that distributed, with the ZK60 alloy phase relatively, dimple is dark, and quantity is many, size has evenly been showed better elongation;
6) add rare-earth element cerium, the heat-resisting Mg mutually of cerium and magnesium formation
12Ce, generally be distributed on the crystal boundary with strip or spherical distribution at intracrystalline, pinning is lived crystal boundary and intracrystalline dislocation motion effectively, becomes the important obstruction that hinders dislocation motion and crystal grain distortion, keep material internal under the high temperature that the dislocation of higher density is arranged, improved the intensity of alloy under the high temperature;
7) add rare-earth element cerium, room temperature average tensile strength 360MPa under the alloy extruding attitude, yield strength 245MPa, elongation after fracture 7%; Average tensile strength 250MPa in the time of 150 ℃, elongation after fracture is greater than 11%.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1:
Will be after magnesium ingot 1116kg, the zinc ingot metal 54kg pre-treatment drop in the off-the-shelf clean crucible, add flux 18kg fusing at the bottom of the RJ-2, be sprinkled into RJ-4 insulating covering agent 3.6kg in the process to prevent burning, magnesium liquid outlet temperature is controlled at 670 ℃, and the time is controlled at 4h; Fusing is warming up to 780 ℃ after finishing, and adds potassium fluotitanate 0.75kg in batches and lentamente and is preheated to 300 ℃ of rare-earth element cerium 30kg, drags for the end and stirs 3min, makes the alloy homogenizing; The alloy liquid temp is adjusted to 750 ℃, and blowing argon gas adds RJ-6 refining agent 18kg refining 6min simultaneously; Refining is warming up to 780 ℃ with alloy liquid and leaves standstill 10min after finishing; Reduce at last under 690 ℃ of temperature condition, and at SF
6Pour into a mould under the protective atmosphere.The weight percent of the chemical composition of the magnesium alloy that makes like this is Zn:4.5%, Ce:2.5%, Ti:0.01%, Si: Fe≤0.08%: Cu≤0.01%: Ni≤0.01%: other impurity elements≤0.002% :≤0.05%, and surplus is Mg.Room temperature average tensile strength 350MPa under its extruding attitude, yield strength 235MPa, elongation after fracture 6.5%; Average tensile strength 240MPa in the time of 150 ℃, elongation after fracture is greater than 11%.
Owing to drag in the process of the end and standing sedimentation at magnesium liquid, have part material and be eliminated, add the reason of high temperature oxidation, the yield rate of making is between 95～96%.Therefore certain composition when sampling analysis, might occur and not meet the predetermined preparation requirement of alloy, at this moment should be according to predetermined prescription, the melting once more of some raw material of corresponding adding is till sampling analysis is qualified.For following embodiment above-mentioned requirement is arranged all.
Embodiment 2:
Will be after magnesium ingot 1121kg, the zinc ingot metal 60kg pre-treatment drop in the off-the-shelf clean crucible, add flux 24kg fusing at the bottom of the RJ-2, be sprinkled into RJ-5 insulating covering agent 4.8kg in the process to prevent burning, magnesium liquid outlet temperature is controlled at 680 ℃, and the time is controlled at 5h; Fusing is warming up to 795 ℃ after finishing, and adds potassium fluotitanate 7.5kg in batches and lentamente and is preheated to 300 ℃ of rare-earth element cerium 18kg, drags for the end and stirs 4min, makes the alloy homogenizing; The alloy liquid temp is adjusted to 755 ℃, and blowing argon gas adds RJ-5 refining agent 24kg refining 8min simultaneously; Refining is warming up to 795 ℃ with alloy liquid and leaves standstill 15min after finishing; Reduce at last under 700 ℃ of temperature condition, and at SO
2Pour into a mould under the protective atmosphere.The weight percent of the chemical composition of the magnesium alloy that makes like this is Zn:5.0%, Ce:1.5%, Ti:0.10%, Si: Fe≤0.08%: Cu≤0.01%: Ni≤0.01%: other impurity elements≤0.002% :≤0.05%, and surplus is Mg.Room temperature average tensile strength 360MPa under its extruding attitude, yield strength 245MPa, elongation after fracture 7.0%; Average tensile strength 250MPa in the time of 150 ℃, elongation after fracture is greater than 11%.
Embodiment 3:
Will be after magnesium ingot 1125.5kg, the zinc ingot metal 66kg pre-treatment drop in the off-the-shelf clean crucible, add flux 30kg fusing at the bottom of the RJ-2, process is sprinkled into RJ-6 insulating covering agent 6.0kg to prevent burning, and magnesium liquid outlet temperature is controlled at 690 ℃, and the time is controlled at 6h; Fusing is warming up to 810 ℃ after finishing, and adds potassium fluotitanate 15kg in batches and lentamente and is preheated to 300 ℃ of rare-earth element cerium 6kg, drags for the end and stirs 5min, makes the alloy homogenizing; The alloy liquid temp is adjusted to 760 ℃, and blowing argon gas adds RJ-4 refining agent 30kg refining 10min simultaneously; Refining is warming up to 810 ℃ with alloy liquid and leaves standstill 20min after finishing; Reduce at last under 710 ℃ of temperature condition, and at CO
2Pour into a mould under the protective atmosphere.The weight percent of the chemical composition of the magnesium alloy that makes like this is Zn:5.5%, Ce:0.5%, Ti:0.20%, Si: Fe≤0.08%: Cu≤0.01%: Ni≤0.01%: other impurity elements≤0.002% :≤0.05%, and surplus is Mg.Room temperature average tensile strength 370MPa under its extruding attitude, yield strength 255MPa, elongation after fracture 7.5%; Average tensile strength 260MPa in the time of 150 ℃, elongation after fracture is greater than 11%.
Claims (2)
1, a kind of Wrought magnesium alloys in high intensity, high plasticity, the weight percent that it is characterized in that component is: Zn:4.5～5.5%, Ce:0.5～2.5%, Ti:0.01～0.20%, Si: Fe≤0.08%: Cu≤0.01%: Ni≤0.01%: other impurity elements≤0.002% :≤0.05%, and surplus is Mg.
2, the preparation method of the described Wrought magnesium alloys in high intensity, high plasticity of claim 1 is characterized in that may further comprise the steps:
1) adds end flux melts with dropping in the off-the-shelf clean crucible after industrial magnesium ingot, the zinc ingot metal pre-treatment, the consumption of end flux accounts for 1.5～2.5% of quality of furnace charge, be sprinkled into insulating covering agent simultaneously, the consumption of insulating covering agent accounts for 0.3～0.5% of quality of furnace charge, the whole melting process time is controlled at 2～6h, and magnesium liquid outlet temperature is controlled at 670～690 ℃;
2) after fusing finishes, be warming up to 780～810 ℃, add potassium fluotitanate and rare-earth element cerium in batches and lentamente, all after the fusing, drag for the end and stir 3～5min, make the alloy homogenizing, wherein rare-earth element cerium is preheated to 300～400 ℃;
3) the alloy liquid temp is adjusted to 750～760 ℃ of blowing argon gas refining 6～10min, adds refining agent simultaneously, the consumption of refining agent accounts for 1.5～2.5% of quality of furnace charge;
4) alloy liquid is warming up to 780～810 ℃ and leaves standstill 10～20min;
5) alloy liquid is reduced under 690～710 ℃ of temperature condition, and under protective atmosphere, pour into a mould;
Flux of the above-mentioned end, insulating covering agent and refining agent are selected for use and are not contained MgCl
2Flux.
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|---|---|---|---|
| CNB2007100222168A CN100457945C (en) | 2007-05-09 | 2007-05-09 | Wrought magnesium alloys in high intensity, high plasticity, and preparation method |
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| CNB2007100222168A CN100457945C (en) | 2007-05-09 | 2007-05-09 | Wrought magnesium alloys in high intensity, high plasticity, and preparation method |
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| CN100457945C true CN100457945C (en) | 2009-02-04 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100584980C (en) * | 2007-12-12 | 2010-01-27 | 中国科学院长春应用化学研究所 | Magnesium-zinc-lanthanon alloy and method for preparing same |
| CN102051509A (en) * | 2010-12-28 | 2011-05-11 | 西安工业大学 | High-toughness heat-resistant Mg-Al-RE-Mn wrought magnesium alloy and preparation method of plate made of same |
| CN102952984B (en) * | 2011-08-29 | 2015-08-26 | 比亚迪股份有限公司 | A kind of wrought magnesium alloys and preparation method thereof |
| CN104099507A (en) * | 2014-07-14 | 2014-10-15 | 沈阳工业大学 | High-strength and high-toughness rare earth magnesium alloy |
| CN104372224B (en) * | 2014-10-20 | 2016-10-05 | 西南交通大学 | A kind of accurate brilliant enhancing complex magnesium alloy and preparation method thereof |
| CN106319314A (en) * | 2016-11-07 | 2017-01-11 | 天津东义镁制品股份有限公司 | High-speed extrusion high-strength deforming magnesium alloy and preparation method thereof |
| CN108823475A (en) * | 2018-08-23 | 2018-11-16 | 中北大学 | A kind of preparation method of the magnesium titanium alloy plate of high rare-earth content |
| CN109136703A (en) * | 2018-09-20 | 2019-01-04 | 贵州大学 | A kind of ZK60 magnesium alloy and preparation method thereof |
| CN109763045A (en) * | 2019-03-22 | 2019-05-17 | 鹤壁恒镁新材料科技有限公司 | Middle high-strength magnesium alloy and preparation method thereof |
| CN112481537A (en) * | 2020-12-09 | 2021-03-12 | 佳威科技(海安)有限公司 | High-strength magnesium alloy material and preparation method thereof |
| CN114182130A (en) * | 2021-12-02 | 2022-03-15 | 上海航天精密机械研究所 | Refining agent for magnesium alloy with high rare earth content, preparation method and application method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996024701A1 (en) * | 1995-02-06 | 1996-08-15 | British Aluminium Holdings Limited | Magnesium alloys |
-
2007
- 2007-05-09 CN CNB2007100222168A patent/CN100457945C/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996024701A1 (en) * | 1995-02-06 | 1996-08-15 | British Aluminium Holdings Limited | Magnesium alloys |
Non-Patent Citations (2)
| Title |
|---|
| Ce对镁及镁合金中晶粒的细化机理. 余琨，黎文献，张世军.稀有金属材料与工程，第34卷第7期. 2005 |
| Ce对镁及镁合金中晶粒的细化机理. 余琨，黎文献，张世军.稀有金属材料与工程，第34卷第7期. 2005 * |
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Address after: 211212 No. 11 Kaiping Road, Dongping Street, Lishui District, Nanjing City, Jiangsu Province Patentee after: Baowu Magnesium Industry Technology Co.,Ltd. Address before: Baizhen Lishui County of Nanjing City, Jiangsu province 211221 Hong Nanjing welbow metals Limited by Share Ltd Patentee before: NANJING YUNHAI SPECIAL METALS Co.,Ltd. |