CN113649416A - Method for promoting precipitation of second phase of magnesium alloy through multidirectional hot rolling and annealing treatment - Google Patents
Method for promoting precipitation of second phase of magnesium alloy through multidirectional hot rolling and annealing treatment Download PDFInfo
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- CN113649416A CN113649416A CN202110828950.3A CN202110828950A CN113649416A CN 113649416 A CN113649416 A CN 113649416A CN 202110828950 A CN202110828950 A CN 202110828950A CN 113649416 A CN113649416 A CN 113649416A
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- magnesium alloy
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 85
- 238000000137 annealing Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000005098 hot rolling Methods 0.000 title claims abstract description 25
- 238000001556 precipitation Methods 0.000 title claims abstract description 25
- 230000001737 promoting effect Effects 0.000 title claims abstract description 14
- 238000005096 rolling process Methods 0.000 claims abstract description 68
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 17
- 239000000956 alloy Substances 0.000 claims abstract description 17
- 238000004321 preservation Methods 0.000 claims abstract description 9
- 238000005728 strengthening Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 238000010899 nucleation Methods 0.000 abstract description 4
- 230000006911 nucleation Effects 0.000 abstract description 4
- 238000009825 accumulation Methods 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 abstract 1
- 238000003672 processing method Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910001200 Ferrotitanium Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003562 lightweight material Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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Classifications
-
- 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
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
- C21D8/0226—Hot rolling
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
-
- 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
Abstract
The invention discloses a method for promoting the precipitation of a second phase of a magnesium alloy through multidirectional hot rolling and annealing treatment, and belongs to the field of metal material processing and forming processes. The method specifically comprises the following steps: and (2) performing multi-pass direction-changing hot rolling on the magnesium alloy plate containing the second phase, sequentially increasing the reduction of each pass, putting the magnesium alloy plate into a heating box for heating and heat preservation between passes, and performing annealing heat treatment on the plate after rolling. The invention promotes the accumulation of dislocation by the multidirectional rolling process with increasing reduction and increases the dislocation density. The high dislocation density provides energy for nucleation of a precipitated phase in the annealing process after heating, heat preservation and rolling among passes, so that the precipitation of a second phase of the magnesium alloy plate is promoted, the alloy precipitation strengthening effect is improved, the growth of crystal grains in the recrystallization process is inhibited, and the mechanical property of the alloy plate is improved. The preparation method is simple, can effectively increase the precipitation strengthening and fine grain strengthening effects of the alloy plate, improves the mechanical property, and has good application prospect.
Description
Technical Field
The invention belongs to the field of metal material processing and forming processes, particularly relates to a processing method for promoting second phase precipitation, and particularly relates to a method for promoting second phase precipitation of magnesium alloy through excessive hot rolling and annealing treatment.
Background
With the increase of the demand of energy conservation and emission reduction, people have more and more demands on lightweight materials. Therefore, the magnesium alloy is expected to be widely applied in the fields of automobiles, electrical appliances and aerospace due to low density, light weight and high specific strength. However, the limited mechanical properties of magnesium alloys at room temperature have greatly limited their further applications.
Precipitation strengthening is one of the most effective strengthening methods for magnesium alloys, and is often used to improve the strength of magnesium alloys. The precipitation strengthening effect is closely related to the density of the precipitated phase, and generally, the strengthening effect is better as the precipitated phase density is higher. Moreover, the precipitated phase can also hinder the movement of a grain boundary, so that the effect of grain refinement is achieved, and the strength of the alloy is further improved. However, for magnesium alloys with low alloy content (the mass fraction content of the added alloy is not more than 8 wt.%), solute atoms are usually dissolved in the magnesium matrix in a solid manner, so that the precipitated phase is less, and the strength of the alloy is limited. The patent provides a processing method, and an effective means is provided for promoting the precipitation of the magnesium alloy plate, refining the crystal grains of the magnesium alloy plate and improving the mechanical property of the magnesium alloy plate.
Disclosure of Invention
The invention provides a method for promoting the precipitation of a second phase of a magnesium alloy through multidirectional hot rolling and annealing treatment, and aims to provide a processing method which is simple in process and beneficial to the precipitation of the second phase in a magnesium alloy plate, so that the prepared magnesium alloy plate has higher precipitated phase density, finer grains and higher strength.
The technical scheme of the invention is as follows:
the method for promoting the precipitation of the second phase of the magnesium alloy specifically comprises the following steps:
(1) heating the roller to 50-250 ℃, and heating the heating box to 150-400 ℃;
(2) placing the magnesium alloy plate into a heating box, standing and preserving heat for 5-30 minutes;
(3) feeding the magnesium alloy plate between rollers to finish single-pass rolling, wherein the reduction is 3-15%;
(4) rotating the magnesium alloy plate by 90 degrees by taking the normal direction of the magnesium alloy plate as an axis and repeating the step (2);
(5) feeding the magnesium alloy plate between rollers to finish the second pass rolling, wherein the reduction is 10-30%;
(6) repeating the step (4);
(7) feeding the magnesium alloy plate between rollers to finish the third rolling, wherein the rolling reduction is 20-45%;
(8) repeating the step (6);
(9) feeding the magnesium alloy plate between rollers to finish the fourth pass of rolling, wherein the reduction is 35-65%;
(10) and placing the rolled plate into a heating oven at the temperature of 200-400 ℃ for heat preservation for 5-60 minutes for annealing treatment.
Wherein, the rotating direction in the step (4) is preferably clockwise.
On the basis of the traditional multi-pass hot rolling process, the plate is rotated by 90 degrees in each pass by taking the normal direction as an axis so as to apply rolling forces in different directions to the plate and promote dislocation accumulation; the reduction of each pass is increased progressively, so as to provide enough nucleation sites for nucleation of precipitated phases in the final annealing process; and promoting the dynamic precipitation and the static precipitation of a second phase by hot rolling, inter-pass heat preservation and annealing, and finally achieving the purpose of improving the density of the precipitated phase of the magnesium alloy.
The invention can carry out rolling for more passes, and only needs to continuously repeat the steps (8) to (9) among the passes and continuously increase the rolling reduction. The total rolling reduction of the multi-directional hot rolling in the invention is 65-95%.
Preferably, the reduction per pass of the rolling increases with the number of passes.
Preferably, the magnesium alloy sheet in step (2) should be selected from magnesium alloy sheets containing a second phase and having an alloy mass fraction content of less than 8 wt.%, such as Mg-2Al-0.8Sn-0.5Ca, Mg-4Al-1Zn, Mg-2Al-1Ca, Mg-2Al-0.3Ca-1.0Sm (wt.%), and the like.
Compared with the prior art, the method has the following beneficial effects:
(1) the invention provides a magnesium alloy processing method which has simple and reliable process, low processing cost and easy realization of large-scale application; the method is an ideal plastic processing method for processing the high-performance magnesium alloy with low cost and short flow;
(2) the rolling process design with the gradually increased multi-directional rolling reduction ensures that the dislocation moving along different directions is easier to start in the rolling process, promotes dislocation entanglement and provides sufficient nucleation sites for the precipitation of precipitated phases;
(3) the rolling process design with the multi-directional incremental rolling reduction ensures that the crystal grains of the magnesium alloy plate can bear rolling force with different and incremental directions in each pass, so that the crystal grains are enabled to shift along different directions, the texture is weakened, and the in-plane anisotropy of the plate is reduced;
(4) the invention can weaken the texture, promote the precipitation of precipitated phase and refine crystal grains, thereby greatly improving the mechanical property of the magnesium alloy plate, and is expected to be applied to the preparation of alloy plates sensitive to precipitation strengthening response, such as aluminum alloy, titanium alloy, steel and the like.
Drawings
FIG. 1 is a schematic view of a multi-directional hot rolling and annealing process
FIG. 2a is a photograph of a back-scattered scan of a Mg-2Al-0.8Sn-0.5Ca (wt.%) alloy sheet of example one which was multi-directionally hot rolled and annealed
FIG. 2b is a photograph of a back-scattered scan of a Mg-2Al-0.8Sn-0.5Ca (wt.%) alloy sheet of example one that was conventionally hot rolled and annealed
FIG. 3a is a TEM photograph of a Mg-2Al-0.8Sn-0.5Ca (wt.%) alloy sheet in example I after multi-directional hot rolling and annealing
FIG. 3b is a TEM photograph of a Mg-2Al-0.8Sn-0.5Ca (wt.%) alloy sheet of example I that was conventionally hot rolled and annealed
FIG. 4 is a room temperature tensile curve of a Mg-2Al-0.8Sn-0.5Ca (wt.%) alloy sheet of example one which is multi-directionally hot rolled and annealed as compared to a conventional hot rolled and annealed sheet
Detailed description of the invention
The technical solution of the invention is further explained and illustrated in the form of specific embodiments.
Example 1
(1) Selecting a magnesium alloy plate with the thickness of 4 mm and the components of Mg-2Al-0.8Sn-0.5Ca (wt.%);
(2) adjusting the roll gap of the roll to 3.4 mm, and respectively raising the temperature of the roll and the temperature of the heating box to 100 ℃ and 300 ℃;
(3) putting the magnesium alloy plate into a heating box, standing and preserving heat for 7 minutes;
(4) feeding the magnesium alloy plate between rollers to finish single-pass rolling, wherein the rolling reduction is 15%;
(5) rotating the magnesium alloy plate clockwise by 90 degrees by taking the normal direction as an axis and repeating the step (3)
(6) Adjusting the roll gap of the rolls to 2.7 mm, and feeding the magnesium alloy plate between the rolls to finish the second pass of rolling, wherein the rolling reduction is 20%;
(7) repeating the step (5);
(8) adjusting the roll gap of the rolls to 1.9 mm, and feeding the magnesium alloy plate between the rolls to finish the third rolling, wherein the rolling reduction is 30%;
(9) repeating the step (7);
(10) adjusting the roll gap of the rolls to 1.0 mm, and feeding the magnesium alloy plate between the rolls to finish the fourth pass of rolling, wherein the rolling reduction is 45 percent, and the total rolling reduction is 75 percent;
(11) and putting the magnesium alloy plate into a heating oven heated to 275 ℃ for heat preservation for 8 minutes for annealing treatment.
The 4 mm alloy sheet was also subjected to a set of conventional hot rolling and annealing treatment experiments as a control, in which the rolling temperature was the same as the reduction and the multi-directional hot rolling.
After multi-directional hot rolling and annealing treatment, the yield strength of the plate is 251MPa, the tensile strength is 302MPa, and the fracture elongation is 23.4 percent; after the conventional hot rolling and annealing treatment, the yield strength of the plate is 210MPa, the tensile strength is 269MPa, the fracture elongation is 20.9 percent, the multidirectional hot rolling and annealing treatment processing method obviously promotes the precipitation of a second phase, and the room-temperature mechanical property of the alloy is obviously improved.
Example 2:
(1) selecting a magnesium alloy plate with the thickness of 5 mm and the component of Mg-4Al-1Zn (wt%);
(2) adjusting the roll gap of the roll to 4.25 mm, and respectively raising the temperature of the roll and the temperature of the heating box to 100 ℃ and 350 ℃;
(3) putting the magnesium alloy plate into a heating box, standing and preserving heat for 6 minutes;
(4) feeding the magnesium alloy plate between rollers to finish single-pass rolling, wherein the rolling reduction is 15%;
(5) rotating the magnesium alloy plate clockwise by 90 degrees by taking the normal direction as an axis and repeating the step (3)
(6) Adjusting the roll gap of the rolls to 3.19 mm, and feeding the magnesium alloy plate between the rolls to finish the second pass of rolling, wherein the rolling reduction is 25%;
(7) repeating the step (5);
(8) adjusting the roll gap of the rolls to 1.91 mm, and feeding the magnesium alloy plate between the rolls to finish the third rolling, wherein the rolling reduction is 40%;
(9) repeating the step (7);
(10) adjusting the roll gap of the rolls to 0.86 mm, and feeding the magnesium alloy plate between the rolls to finish the fourth pass of rolling, wherein the rolling reduction is 55 percent, and the total rolling reduction is 73 percent;
(11) and putting the magnesium alloy plate into a heating oven heated to 275 ℃ for heat preservation for 30 minutes for annealing treatment.
After multi-directional hot rolling and annealing treatment, the yield strength of the plate is 233MPa, the tensile strength is 286MPa, and the elongation at break is 24.2 percent.
Example 3:
(1) selecting a magnesium alloy plate with the thickness of 6 millimeters and the component of Mg-2Al-1Ca (wt.%);
(2) adjusting the roll gap of the roll to 5.40 mm, and respectively raising the temperature of the roll and the temperature of the heating box to 100 ℃ and 300 ℃;
(3) putting the magnesium alloy plate into a heating box, standing and preserving heat for 5 minutes;
(4) feeding the magnesium alloy plate between rollers to finish single-pass rolling, wherein the rolling reduction is 10%;
(5) rotating the magnesium alloy plate clockwise by 90 degrees by taking the normal direction of the magnesium alloy plate as an axis and repeating the step (3);
(6) adjusting the roll gap of the rolls to 4.59 mm, and feeding the magnesium alloy plate between the rolls to finish the second pass of rolling, wherein the rolling reduction is 15%;
(7) repeating the step (5);
(8) adjusting the roll gap of the rolls to 3.67 mm, and feeding the magnesium alloy plate between the rolls to finish the third rolling, wherein the rolling reduction is 20%;
(9) repeating the step (7);
(10) adjusting the roll gap of the rolls to 2.75 mm, and feeding the magnesium alloy plate between the rolls to finish the fourth pass of rolling, wherein the rolling reduction is 25%;
(11) repeating the step (9);
(12) adjusting the roll gap of the rolls to 1.93 mm, and feeding the magnesium alloy plate between the rolls to finish the fifth pass of rolling, wherein the rolling reduction is 30%;
(13) repeating the step (11);
(14) adjusting the roll gap of the rolls to 1.25 mm, and feeding the magnesium alloy plate between the rolls to finish the sixth pass of rolling, wherein the rolling reduction is 35 percent, and the total rolling reduction is 79.1 percent;
(15) and putting the magnesium alloy plate into a heating oven heated to 250 ℃ for heat preservation for 25 minutes for annealing treatment.
After multi-directional hot rolling and annealing treatment, the yield strength of the plate is 253MPa, the tensile strength is 307MPa, and the elongation at break is 16.7 percent.
Example 4:
(1) selecting a magnesium alloy plate with the thickness of 5 mm and the components of Mg-2Al-0.3Ca-0.6Sm (wt.%);
(2) adjusting the roll gap of the roll to 4.50 mm, and respectively raising the temperature of the roll and the temperature of the heating box to 100 ℃ and 275 ℃;
(3) putting the magnesium alloy plate into a heating box, standing and preserving heat for 10 minutes;
(4) feeding the magnesium alloy plate between rollers to finish single-pass rolling, wherein the rolling reduction is 10%;
(5) rotating the magnesium alloy plate clockwise by 90 degrees by taking the normal direction of the magnesium alloy plate as an axis and repeating the step (3);
(6) adjusting the roll gap of the rolls to 3.60 mm, and feeding the magnesium alloy plate between the rolls to finish the second pass of rolling, wherein the rolling reduction is 20%;
(7) repeating the step (5);
(8) adjusting the roll gap of the rolls to 2.34 mm, and feeding the magnesium alloy plate between the rolls to finish the third rolling, wherein the rolling reduction is 35%;
(9) repeating the step (7);
(10) adjusting the roll gap of the rolls to 1.17 mm, and feeding the magnesium alloy plate between the rolls to finish the fourth pass of rolling, wherein the rolling reduction is 50 percent, and the total rolling reduction is 76.6 percent;
(11) and putting the magnesium alloy plate into a heating oven heated to 250 ℃ for heat preservation for 20 minutes for annealing treatment.
After multi-directional hot rolling and annealing treatment, the yield strength of the plate is-216 MPa, the tensile strength is-271 MPa, and the elongation at break is-18.6%.
Claims (6)
1. A method for promoting the precipitation of a second phase of a magnesium alloy by multi-directional hot rolling and annealing treatment, which is characterized by comprising the following steps:
(1) heating the roller to 50-250 ℃, and heating the heating box to 150-400 ℃;
(2) placing the magnesium alloy plate into a heating box, standing and preserving heat for 5-30 minutes;
(3) feeding the magnesium alloy plate between rollers to finish single-pass rolling, wherein the reduction is 3-15%;
(4) rotating the magnesium alloy plate by 90 degrees by taking the normal direction of the magnesium alloy plate as an axis and repeating the step (2);
(5) feeding the magnesium alloy plate between rollers to finish the second pass rolling, wherein the reduction is 10-30%;
(6) repeating the step (4);
(7) feeding the magnesium alloy plate between rollers to finish the third rolling, wherein the rolling reduction is 20-45%;
(8) repeating the step (6);
(9) feeding the magnesium alloy plate between rollers to finish the fourth pass of rolling, wherein the reduction is 35-65%;
(10) and placing the rolled plate into a heating oven at the temperature of 200-400 ℃ for heat preservation for 5-60 minutes for annealing treatment.
2. A method for promoting the precipitation of a second phase of a magnesium alloy by multi-directional hot rolling and annealing, characterized in that the rotation direction in the step (4) is preferably clockwise.
3. The method of claim 1, wherein the second phase of the magnesium alloy is precipitated by the multi-pass hot rolling and annealing treatment, and the method comprises repeating the rolling in more passes and successively increasing the reduction to a total rolling reduction of 65 to 95%.
4. The method of promoting the precipitation of the second phase of the magnesium alloy by the multi-pass hot rolling and annealing process as claimed in claim 1, wherein the reduction per pass of the rolling is increased with the number of passes.
5. The method for promoting the precipitation of the second phase of the magnesium alloy by the multi-hot rolling and annealing treatment as claimed in claim 1, wherein the magnesium alloy sheet in the step (2) is selected from magnesium alloy sheets containing the second phase and having an alloy mass fraction content of less than 8 wt.%.
6. The method for promoting the precipitation of the second phase of the magnesium alloy by the multi-hot rolling and annealing treatment as recited in claim 5, wherein the magnesium alloy sheet is Mg-2Al-0.8Sn-0.5Ca, Mg-4Al-1Zn, Mg-2Al-1Ca or Mg-2Al-0.3Ca-1.0 Sm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115747685A (en) * | 2022-11-18 | 2023-03-07 | 哈尔滨工程大学 | Low-density high-specific-strength beta-phase magnesium-lithium alloy prepared based on deep cooling polyhedral rolling and preparation method |
| CN116200637A (en) * | 2023-01-06 | 2023-06-02 | 吉林大学 | Magnesium alloy with high formability and low rare earth content at room temperature and preparation method thereof |
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| CN116200637A (en) * | 2023-01-06 | 2023-06-02 | 吉林大学 | Magnesium alloy with high formability and low rare earth content at room temperature and preparation method thereof |
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