CN114196859A - Method for preparing nanocrystalline-containing high-lithium magnesium lithium alloy by rolling at room temperature - Google Patents
Method for preparing nanocrystalline-containing high-lithium magnesium lithium alloy by rolling at room temperature Download PDFInfo
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- 238000005096 rolling process Methods 0.000 title claims abstract description 48
- 229910000733 Li alloy Inorganic materials 0.000 title claims abstract description 37
- 239000001989 lithium alloy Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 20
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 45
- 239000000956 alloy Substances 0.000 claims abstract description 45
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000011777 magnesium Substances 0.000 claims abstract description 17
- 238000001953 recrystallisation Methods 0.000 claims abstract description 11
- 238000000265 homogenisation Methods 0.000 claims abstract description 9
- 230000006911 nucleation Effects 0.000 claims abstract description 9
- 238000010899 nucleation Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 230000009467 reduction Effects 0.000 claims description 14
- 229910052744 lithium Inorganic materials 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 230000005501 phase interface Effects 0.000 claims description 7
- 230000006698 induction Effects 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 238000005275 alloying Methods 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- WWKWZYPOPJIVGF-UHFFFAOYSA-N [Li].[Li].[Mg] Chemical compound [Li].[Li].[Mg] WWKWZYPOPJIVGF-UHFFFAOYSA-N 0.000 claims 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 14
- 239000007788 liquid Substances 0.000 abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 7
- 238000012545 processing Methods 0.000 abstract description 6
- 238000013461 design Methods 0.000 abstract description 3
- 229910000861 Mg alloy Inorganic materials 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000002159 nanocrystal Substances 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000002301 combined effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005303 weighing Methods 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2200/00—Crystalline structure
- C22C2200/04—Nanocrystalline
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- Materials Engineering (AREA)
- Metallurgy (AREA)
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Abstract
The invention provides a method for preparing a nanocrystalline high-lithium magnesium lithium alloy by rolling at room temperature, which belongs to the technical field of magnesium lithium alloy processing, and comprises the following steps of 1) selecting a high-lithium-content single-phase beta (Li) alloy to play the ultralight characteristic of the alloy, 2) carrying out homogenization pretreatment on an as-cast alloy to separate out an Alfa (Mg) phase from the beta (Li) phase, and 3) rolling the homogenized alloy at room temperature. The invention introduces a large amount of alpha/beta phase boundaries as recrystallization nucleation sites through homogenization treatment, promotes dynamic recrystallization nucleation, overcomes the technical obstacle that the magnesium-lithium alloy can only be cooled and rolled by liquid nitrogen to generate nanocrystalline, adopts simple heat treatment and room temperature rolling processes, and finally obtains the nanocrystalline with the strength of more than 225MPa and the density of 1.44g/cm3The magnesium-lithium alloy with the grain size of 45-110nm has great microstructure design directivity.
Description
Technical Field
The invention belongs to the field of magnesium-lithium alloy processing, and particularly relates to a method for preparing a nanocrystalline high-lithium magnesium-lithium alloy by rolling at room temperature.
Background
The magnesium-lithium alloy is the lightest metal structure material in the world at present, and has the characteristics of high specific strength, good damping and shock absorption performance, excellent electromagnetic shielding performance and the like. The method has an irreplaceable position in lightweight design in the aerospace field.
For magnesium alloy, due to the fact that Hall-Petch coefficient of the magnesium alloy is large, grain refinement is an effective means for improving mechanical properties of the alloy, and particularly fine-grain magnesium alloy with a nanoscale size has excellent mechanical properties. However, for magnesium-lithium alloys, especially for high lithium content magnesium-lithium alloys, the dynamic recrystallization temperature is very low, dynamic recrystallization can occur even during room temperature plastic deformation, and recrystallized grains are easily grown to micron-level grains, thereby reducing the mechanical properties of the processed shapes. Therefore, the nanocrystalline magnesium-lithium alloy can be prepared by inhibiting the growth of crystal grains only by processing under the condition of liquid nitrogen cooling. However, the formability of the alloy is deteriorated under the liquid nitrogen condition, which easily causes cracking of the processed profile, and the use of liquid nitrogen also increases the manufacturing cost of the alloy, which makes industrial popularization difficult. Therefore, obtaining the nanocrystalline magnesium-lithium alloy at room temperature is one of the keys for popularizing the industrial production of the high-performance magnesium-lithium alloy.
The patent discloses a method for preparing a twin-crystal magnesium alloy with ultrahigh strength and toughness and nanometer gradient through searching documents in the prior art, the magnesium alloy is enabled to be in a hydrostatic pressure of 5-8 GPa under the action of a pressure head through a high-pressure torsion method, then an upper die and a lower die rotate, the number of torsion turns is 8-12 times, and then the magnesium alloy subjected to severe plastic deformation is subjected to aging treatment.
Further literature search found that Siyuan Jin et al, Materials Science and Engineering, A: a, 788(2020) (139611), published "Combination effects of Yb addition and cryogenic-rolling on microstructure and mechanical properties of LA141 alloy" (the combined effect of Yb addition and cryogenic rolling on the structure and performance of LA141 alloy) in the text, the massive nanocrystalline magnesium-lithium alloy is prepared under the condition of liquid nitrogen cooling, and is suitable for preparation and processing of magnesium-lithium alloy plates.
Aiming at the defects in the prior art, the invention provides a method for preparing nanocrystalline magnesium-lithium alloy by rolling at room temperature, and provides an effective way for industrialized mass production of nanocrystalline magnesium-lithium alloy.
Disclosure of Invention
The purpose of the invention is as follows: a large number of recrystallization nucleation sites are provided by introducing a large number of phase interfaces through homogenization, and recrystallized grains are refined through discontinuous dynamic recrystallization, so that nanocrystals are formed through rolling at room temperature, and the technical obstacle that the nanocrystals can be generated only through liquid nitrogen cooling rolling of the magnesium-lithium alloy is overcome.
The technical scheme of the invention is as follows:
a method for preparing a nanocrystalline high-lithium magnesium lithium alloy by rolling at room temperature comprises the following steps:
(1) selecting a magnesium-lithium alloy: Mg-Li-Ni, the mass percent of each element in the alloy is as follows: li is more than or equal to 11 wt.%, Ni is 0.1-1%, and the balance is Mg;
(2) putting industrial pure Mg, industrial pure Li and Mg-20% Ni intermediate alloy into a vacuum induction melting furnace, filling Ar gas for protection, heating until the alloy is completely melted, and finally adopting a metal mold for casting and molding;
(3) putting the as-cast alloy into a muffle furnace for homogenization treatment at the temperature of 200 ℃ for 10h, and putting the alloy into water for quenching after heat preservation so as to separate out a large amount of Alfa (Mg) phases in a beta (Li) matrix phase and introduce a large amount of phase interfaces;
(4) rolling the homogenized magnesium-lithium alloy at room temperature, wherein the rolling rate is 0-1mm/min, the rolling reduction of each pass is 0-5mm, the total rolling reduction is controlled to be 70-90%, and when dynamic recrystallization occurs in the plastic deformation process, an Alfa (Mg)/beta (Li) phase interface in the alloy serves as a nucleation point and prevents grains from growing.
Furthermore, the rolling speed is 0.5mm/min, the rolling reduction of each pass is 1mm, and the total rolling reduction is 80%;
further, the mass percent of Li is 14%;
furthermore, the alloying elements in the magnesium-lithium alloy can be Al, Zn, rare earth, Sn and Ca besides Ni.
Compared with the existing nanocrystalline magnesium alloy processing technology, the invention has the following advantages:
the ultra-light magnesium-lithium alloy is selected, and the density of the alloy adopted by the invention is only 1.43-1.44g/cm315% lighter than pure magnesium.
The production cost is low: compared with the conventional severe plastic deformation and deep cooling rolling for producing the nanocrystalline magnesium alloy, the invention has the advantages that the rolling is carried out at room temperature, the cost is greatly saved, and the method is suitable for industrial mass production.
Drawings
FIG. 1 is a TEM image of homogenized Mg-14Li-0.5Ni in the example of the present invention;
FIG. 2 is a TEM image of rolled Mg-14Li-0.5Ni in the example of the present invention.
FIG. 3 is a drawing curve of Mg-14Li-0.5Ni in the as-cast and as-rolled states in an example of the present invention;
from microscopic image analysis, it is known that the reason why the rolled alloy forms the nanocrystals is that a large amount of α/β phase interfaces are generated during homogenization treatment, a large amount of nucleation sites are provided for the dynamically recrystallized grains and the growth of the recrystallized grains is hindered, so that the nanocrystals are generated, thereby improving the strength of the rolled alloy.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, but the scope of protection of the present patent is not limited to the embodiments, and any modification made on the basis of the embodiments is within the scope of protection of the present patent.
Example 1:
the method comprises the following steps: the casting process comprises the steps of firstly putting an iron mold into a muffle furnace, preheating and drying for 5 hours at the temperature of 200 ℃, then taking out the iron mold for later use, weighing 140g of Li blocks, 840g of Mg blocks and 25g of Mg-20% Ni intermediate alloy, putting the crucible into an induction melting furnace, vacuumizing the induction melting furnace, then introducing Ar gas for protection, heating the crucible until all metal blocks are melted, preserving heat for 5 minutes, and pouring melted metal liquid into the iron mold to be solidified into cast alloy.
Step two: homogenizing, namely putting the cast alloy into a muffle furnace with Ar gas shield, heating to 200 ℃, preserving heat for 10h, then quenching in water to obtain homogenized alloy, cutting the homogenized alloy into metal blocks with the length of 6cm, the width of 4cm and the height of 1cm by using an electric spark linear cutting machine, and finally polishing the metal blocks by using No. 350 abrasive paper.
Step three: and (4) rolling, namely rolling the alloy block obtained in the step two at room temperature, wherein the rolling speed is 0.5mm/min, the rolling reduction of each pass is 1mm, and the total rolling reduction is 80%.
Example 2:
the method for preparing the nanocrystalline-containing high-lithium-content magnesium-lithium alloy by room temperature rolling comprises the following steps:
(1) smelting Mg-xLi-Mx alloy by a vacuum induction smelting furnace, wherein x is more than or equal to 11 wt.%, and Mx points to some common alloying elements (such as Al, Zn, rare earth, Sn, Ni, Ca and the like) added in the high-lithium-content magnesium-lithium alloy, in the smelting process, Mg and Li both adopt industrial pure Mg and industrial pure Li, and other alloying elements are added in the form of industrial pure metal or in the form of intermediate alloy.
(2) And (3) rolling the homogenized alloy in the step one at room temperature, wherein the rolling speed is 0-1mm/min, the rolling reduction of each pass is 0-5mm, and the total rolling reduction is controlled to be 70-90%. During dynamic recrystallization during plastic deformation, the Alfa (Mg)/beta (Li) phase interface within the alloy acts as a nucleation site and hinders grain growth.
Example 3:
(1) selecting Mg-Li-Ni alloy, wherein the mass percent of each element in the alloy is as follows: 14 percent of Li, 0.1 to 1 percent of Ni and the balance of Mg;
(2) putting industrial pure Mg, industrial pure Li and Mg-20% Ni intermediate alloy into a vacuum induction melting furnace, filling Ar gas for protection, heating until the alloy is completely melted, and finally adopting a metal mold for casting and molding;
(3) placing the as-cast alloy into a muffle furnace for homogenization treatment at 200 ℃ for 10h, and then placing the alloy into water for quenching after heat preservation;
(4) and (3) rolling the homogenized magnesium-lithium alloy at room temperature, wherein the rolling speed is 0.5mm/min, the rolling reduction per pass is 1mm, and the total rolling reduction is 80%.
The invention relates to a method for preparing a nanocrystalline high-lithium magnesium lithium alloy by rolling at room temperature, which belongs to the technical field of magnesium lithium alloy processing, and adopts the technical scheme that 1) a single-phase beta (Li) alloy with high lithium content is selected to exert the ultra-light characteristic of the alloy, 2) cast alloy is subjected to homogenization pretreatment to separate out an Alfa (Mg) phase from the beta (Li) phase, and 3) the homogenized alloy is rolled at room temperature. According to the invention, a large amount of alpha/beta phase boundaries are introduced as recrystallization nucleation sites through homogenization treatment, dynamic recrystallization nucleation is promoted, and the technical obstacle that the magnesium-lithium alloy can only be cooled and rolled by liquid nitrogen to generate nanocrystalline is overcome. Compared with the prior art, the invention adopts simple heat treatment and room temperature rolling process, and finally obtains the product with the strength of more than 225MPa and the density of 1.44g/cm3The magnesium-lithium alloy with the grain size of 45-110nm has great microstructure design directivity. Greatly saves the production cost and is suitable for the industrialized mass production of the nanocrystalline magnesium-lithium alloy.
Claims (4)
1. A method for preparing a nanocrystalline high-lithium magnesium lithium alloy by rolling at room temperature is characterized by comprising the following steps:
(1) selecting a magnesium-lithium alloy: Mg-Li-Ni, the mass percent of each element in the alloy is as follows: li is more than or equal to 11 wt.%, Ni is 0.1-1%, and the balance is Mg;
(2) putting industrial pure Mg, industrial pure Li and Mg-20% Ni intermediate alloy into a vacuum induction melting furnace, filling Ar gas for protection, heating until the alloy is completely melted, and finally adopting a metal mold for casting and molding;
(3) putting the as-cast alloy into a muffle furnace for homogenization treatment at the temperature of 200 ℃ for 10h, and putting the alloy into water for quenching after heat preservation so as to separate out a large amount of Alfa (Mg) phases in a beta (Li) matrix phase and introduce a large amount of phase interfaces;
(4) rolling the homogenized magnesium-lithium alloy at room temperature, wherein the rolling rate is 0-1mm/min, the rolling reduction of each pass is 0-5mm, the total rolling reduction is controlled to be 70-90%, and when dynamic recrystallization occurs in the plastic deformation process, an Alfa (Mg)/beta (Li) phase interface in the alloy serves as a nucleation point and prevents grains from growing.
2. The method for preparing the nanocrystalline lithium-magnesium-lithium-containing alloy by room temperature rolling according to claim 1, wherein the rolling speed is 0.5mm/min, the rolling reduction per pass is 1mm, and the total rolling reduction is 80%.
3. The method for preparing the nanocrystalline lithium-magnesium-lithium-containing alloy by rolling at room temperature according to claim 1, wherein the mass percentage of Li is 14%.
4. The method for preparing the nanocrystalline high-lithium magnesium-lithium alloy by room temperature rolling according to claim 1, wherein the alloying elements in the magnesium-lithium alloy can be Al, Zn, rare earth, Sn and Ca besides Ni.
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| CN114807703A (en) * | 2022-03-25 | 2022-07-29 | 哈尔滨工程大学 | Preparation method of high-strength high-plasticity magnesium-lithium alloy based on high solid solution content |
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| CN106676351A (en) * | 2016-11-29 | 2017-05-17 | 哈尔滨工程大学 | Erbium strengthened magnesium-lithium alloy and preparation method thereof |
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2021
- 2021-12-17 CN CN202111554458.8A patent/CN114196859A/en active Pending
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| Title |
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| HONGYU LIU: "Effect of cryogenic rolling process on microstructure and mechanical properties of Mg-14Li-1Al alloy", 《MATERIALS CHARACTERIZATION》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114807703A (en) * | 2022-03-25 | 2022-07-29 | 哈尔滨工程大学 | Preparation method of high-strength high-plasticity magnesium-lithium alloy based on high solid solution content |
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Inventor after: Wu Ruizhi Inventor after: Zhang Shun Inventor after: Jia Haoyang Inventor after: Du Chunlin Inventor after: Sun Dongpeng Inventor after: Yang Zhenzhao Inventor before: Wu Ruizhi Inventor before: Zhang Shun Inventor before: Du Chunlin Inventor before: Sun Dongpeng Inventor before: Yang Zhenzhao |
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Application publication date: 20220318 |
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