WO2017101710A1 - 镁合金板材的轧制及制备方法 - Google Patents

镁合金板材的轧制及制备方法 Download PDF

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WO2017101710A1
WO2017101710A1 PCT/CN2016/108674 CN2016108674W WO2017101710A1 WO 2017101710 A1 WO2017101710 A1 WO 2017101710A1 CN 2016108674 W CN2016108674 W CN 2016108674W WO 2017101710 A1 WO2017101710 A1 WO 2017101710A1
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rolling
magnesium alloy
pass
alloy sheet
temperature
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PCT/CN2016/108674
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English (en)
French (fr)
Inventor
徐世伟
唐伟能
聂建峰
边明哲
蒋浩民
张丕军
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宝山钢铁股份有限公司
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Priority to KR1020207010125A priority Critical patent/KR102224687B1/ko
Priority to EP16874767.3A priority patent/EP3391976B1/en
Priority to US15/780,476 priority patent/US11534806B2/en
Priority to AU2016372756A priority patent/AU2016372756B2/en
Priority to KR1020187015582A priority patent/KR20180079409A/ko
Priority to JP2018528267A priority patent/JP6792617B2/ja
Publication of WO2017101710A1 publication Critical patent/WO2017101710A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
    • B21B1/24—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process
    • B21B1/26—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process by hot-rolling, e.g. Steckel hot mill
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
    • B21B1/227—Surface roughening or texturing
    • 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
    • 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
    • B21B3/003—Rolling non-ferrous metals immediately subsequent to continuous casting, i.e. in-line rolling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
    • B21B37/46—Roll speed or drive motor control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
    • B21B37/74—Temperature control, e.g. by cooling or heating the rolls or the product
    • 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
    • C21D8/0231—Warm rolling
    • 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
    • C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
    • 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
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
    • B21B2001/225—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length by hot-rolling
    • 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
    • B21B2003/001—Aluminium or its alloys
    • 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

Definitions

  • the invention relates to a non-ferrous metal processing technology, in particular to a rolling process for a magnesium alloy sheet.
  • magnesium alloy is an emerging metal structural material with abundant resources worldwide.
  • the density of magnesium is only 1.74 g/cm 3 , which is only 2/3 of the density of aluminum and 1/4 of the density of steel. This feature makes magnesium alloys have a very broad application prospect in the automotive, aerospace, defense military, electronic communications, and home appliances fields. Rolling as an important means of plastic deformation processing of metal materials has been greatly developed.
  • the application of existing magnesium alloy sheets is still very limited, and its production and usage are far less than steel and other non-ferrous metals (such as aluminum and copper). How to overcome various constraints and widely extend it to related fields for manufacturing is a major issue for the further development of magnesium alloys.
  • magnesium alloy is a close-packed hexagonal crystal structure with few independent slip systems and poor room temperature processing performance. Therefore, the production of magnesium alloy sheet in the prior art is made. It is carried out at a high temperature (hot rolling) by means of multi-pass and small reduction, and it takes more than ten passes to roll the magnesium alloy plate in the existing conventional process.
  • the single pass reduction of the rolled magnesium alloy sheet is generally small (the single pass reduction is usually less than 30%), which is much smaller than the single pass reduction of steel, aluminum, copper and other non-ferrous metals. This results in a large number of rolling processes, high production costs, and low production efficiency.
  • magnesium alloys decreases with increasing strain rate, so the rolling speed usually used during rolling (rolling speed is usually less than 5 m/min) is also much smaller than steel and aluminum and copper.
  • rolling speed is usually less than 5 m/min
  • it will also increase the production cost of magnesium alloy sheets and reduce the production efficiency of magnesium alloy sheets.
  • mechanical properties of magnesium alloy sheets are poor, especially the strength and ductility of magnesium alloy sheets need to be further improved.
  • the publication number is CN101648210A, and the publication date is February 17, 2010.
  • the Chinese patent document entitled "Crystal Processing Method for Low Temperature, High Speed and Large Processing Rolling Deformed Magnesium Alloy Sheet” discloses a method for Processing method of magnesium alloy sheet.
  • the processing method comprises the following steps: in the traditional ingot (slab) ⁇ milling (milling) ⁇ flaw detection ⁇ homogenization treatment ⁇ heating ⁇ hot rolling ⁇ straightening ⁇ sawing ⁇ surface treatment ⁇ detection ⁇ oil coating Based on the process of slab heating-hot rolling production of medium and heavy plates, the rolling temperature and rolling speed (especially the finishing rolling temperature and speed) and the reduction of each pass are used for the hot rolling process in the process.
  • the secondary control is between 8 and 10, and the interval between the deformations of each pass and the cooling rate are used to control the grain size of the hot-rolled magnesium alloy sheet to improve its comprehensive mechanical properties.
  • the processing steps of the processing method are complicated, and the rolling speed is as high as 180 m/min, making it difficult to widely use in actual production.
  • the maximum single-pass processing rate is only 30 to 42%, the single-pass reduction is small, and the processing efficiency of the pass is not high.
  • the Chinese patent document entitled "Preparation Method of a Wide Magnesium Alloy Sheet” discloses a method for efficiently preparing a wide-magnesium alloy sheet.
  • the preparation method comprises the steps of: homogenizing the fine-grained, homogeneous and low internal stress magnesium alloy slab to perform reversible high-speed hot rolling, and adopting intermediate pass high temperature pre-annealing in the reversible high-speed hot rolling process;
  • the sheet is subjected to super large deformation deformation in combination with vertical roll rolling and pre-stretching.
  • a medium thickness plate of magnesium alloy can be obtained, and the above method is used to obtain the cutting head and shear of the medium and thick plate.
  • the surface is polished and polished, after the heating and annealing, the finish rolling, the intermediate pass high temperature pre-annealing is used in the finishing rolling pass, and the plate is super-large combined with repeated bending deformation and high-speed asynchronous rolling. Deformation is performed to obtain a high-precision magnesium alloy sheet.
  • the rolling speed in the processing method disclosed in the Chinese patent document is too fast, and there is a certain safety hazard. At the same time, the process steps of the processing method are complicated and difficult to be widely applied in actual production.
  • the existing magnesium alloy sheet preparation method can not effectively balance the improvement of production efficiency, production cost and mechanical properties.
  • the existing magnesium alloy sheet preparation method is either the rolling speed is too high, or the rolling speed is too low, and the process is complicated, it does not have the feasibility of large-scale industrial production. To this end, companies need to obtain a rolling process that can meet the market demand for magnesium alloy sheet applications.
  • the rolling speed and the pass reduction of the rolling process are appropriate, and can be widely extended to related production and manufacturing fields.
  • the rolling pass of the rolling process is properly controlled, which advantageously improves the rolling efficiency.
  • the use of the rolling process of the present invention can effectively improve the mechanical properties of the sheet, and in particular, can greatly improve the strength and ductility of the sheet.
  • the present invention provides a high-efficiency rolling process for a high-strength and high-ductility magnesium alloy sheet, which is a process for rolling a rolled billet, and the parameter control of the rolling process is: rolling
  • the rolling speed of the pass is 10 to 50 m/min, and the reduction of each rolling pass is controlled to 40 to 90%.
  • the billet is preheated before rolling in each rolling pass, and each rolling pass is controlled.
  • the preheating temperature and rolling temperature before the system are both 250-450 °C.
  • the reduction amount of each rolling pass may be the same or different in the above range.
  • Magnesium alloy materials can obtain better mechanical properties through grain refinement. That is to say, grain refinement can not only improve the processing plasticity of magnesium alloy materials, but also increase the strength of magnesium alloy materials and reduce their mechanics. Anisotropy of performance. Compared with other alloy materials such as iron and aluminum, since the magnesium alloy material has a larger K-factor of the Hall-Petch relationship, the grain refining effect contributes more to the improvement of the strength of the magnesium alloy material. In order to further improve the strength and toughness of magnesium alloys and other mechanical properties, it is necessary to obtain a finer grain structure.
  • the coarse grains and the coarse second phase in the as-cast microstructure are gradually broken and refined, so that the second phase is dispersed and distributed in the magnesium matrix, thereby making the mechanics of the magnesium alloy
  • the performance is further improved to achieve higher strength and better plasticity.
  • the microstructure characteristics of the rolled magnesium alloy sheet such as grain size, texture, etc., and the rolling speed in the rolling process, the single pass reduction (especially the final rolling reduction), the rolling temperature, Annealing temperature and annealing time are closely related.
  • the rolling speed of the magnesium alloy material is fast, the deformation heat generated by the deformation and the frictional heat generated by the contact between the rolling stock and the roll will cause the actual temperature of the rolling stock to rise, and start more deformation modes to improve the alloy.
  • the deformability is such that more dislocations are introduced into the microstructure of the magnesium alloy sheet, dynamic recrystallization is induced, and the deformed grains are refined to obtain a finer magnesium alloy sheet having a smaller crystal grain.
  • Deformation is the source of the driving force that causes the plate to recrystallize.
  • the amount of reduction determines the degree of deformation and the amount of deformation energy, which affects the nucleation rate of static recrystallization, and finally determines the size of static recrystallized grains.
  • a larger amount of deformation can introduce more distortion energy into the microstructure of the magnesium alloy to lower the initial temperature of dynamic recrystallization, which is more favorable for obtaining a finer microstructure in the magnesium alloy sheet.
  • the use of faster rolling speed and larger rolling The rolling process combined with the reduction amount can not only effectively obtain the fine crystal structure, but also improve the mechanical properties of the magnesium alloy sheet, and can also advantageously improve the working efficiency of the rolling.
  • the rolling speed mainly affects the deformation rate.
  • the effect of deformation rate on rolling speed is mainly manifested in two aspects: on the one hand, the deformation rate will affect the actual rolling temperature of the rolled part during the deformation process; on the other hand, the deformation rate will affect the startable deformation mode during the rolling process. These two aspects will comprehensively determine the final rollability of the rolled product at a particular rolling temperature.
  • the inventors have found that in the actual production process, when the rolling speed is 12.1 m/min, the single pass reduction can reach 60% at an appropriate rolling temperature, and with the occurrence of dynamic recrystallization, Increasing the rolling speed can not only effectively improve the rolling ability of the magnesium alloy sheet, but also realize the application of the large reduction rolling. However, if the rolling speed is too fast, the deformation heat generated by the deformation and the frictional heat generated by the contact between the rolling stock and the roll may cause a substantial increase in the actual temperature of the rolled product due to the rolling temperature of the rolled product (ie, the dynamic recrystallization temperature).
  • the rolling speed should not exceed 50 m/min.
  • the deformation heat generated by the deformation and the frictional heat generated by the contact between the rolled piece and the roll are insufficient to cause an increase in the actual temperature of the rolled piece, and instead, due to the contact of the preheated rolled piece with the normal temperature roll. Part of the heat of the rolled product is lost, so that slow rolling cannot achieve rolling with a large reduction.
  • the magnesium alloy sheet has a higher dislocation density, which provides a greater driving force for static recrystallization nucleation, thereby effectively refining.
  • Grains increase the strength and ductility of the sheet.
  • the inventors have also found that the reduction of each pass has an important influence on the microstructure of the magnesium alloy sheet. As the amount of reduction increases, the intragranular dislocation density of the magnesium alloy sheet increases, the lattice distortion increases, and the number of recrystallized grains nucleation increases, thereby allowing the crystal grains in the sheet to be greatly refined.
  • the single pass reduction of each rolling pass in the high-efficiency rolling process of the high-strength and high-ductility magnesium alloy sheet according to the present invention is not less than 40% and not more than 90%.
  • the reduction amount of each rolling pass in the above technical solution is controlled to be between 40% and 90%, the reduction amount per pass becomes larger, and therefore, compared with the existing rolling process In the rolling process of the present invention, fewer rolling passes are experienced, the process steps are simpler, the required rolling time is more economical, and the working efficiency is higher.
  • the preheating temperature and the rolling temperature before rolling of each rolling pass are controlled to be between 250 and 450 ° C. The reason is that the temperature is too high and the grains are high in temperature before and after rolling. The rapid growth underneath reduces the effect of refining the grains by rolling deformation; if the temperature is too low, the plastic deformation ability of the material is low, the rolled sheet is easily cracked, and even the raw material is broken.
  • the preheating time before rolling in each rolling pass is controlled to be 1 to 15 min.
  • Another object of the present invention is to provide a method for preparing a high strength and high ductility magnesium alloy sheet.
  • a magnesium alloy sheet having high strength and good ductility can be obtained by the preparation method.
  • the preparation method has simple process steps, requires less time, and has high production efficiency.
  • the method for preparing a high-strength and high-ductility magnesium alloy sheet according to the present invention has a low production cost and can be widely extended to related production and manufacturing fields.
  • the present invention provides a method for preparing a high strength and high ductility magnesium alloy sheet, which comprises the steps of:
  • the preheating time before rolling in each rolling pass is controlled to be 1 to 15 min.
  • the rolling single pass reduction and the rolling temperature are not It can only effectively improve the mechanical properties of the magnesium alloy sheet, and can advantageously improve the rolling efficiency of the magnesium alloy sheet. Since the design principle of controlling the rolling process parameters has been described in detail above, the design principle of the parameter control of the above hot rolling process will not be described again.
  • the reduction amount of each rolling pass in the high-efficiency hot rolling is controlled to be 40 to 90%, that is, compared with the rolling reduction amount used in the prior art, The amount of reduction per pass becomes larger, and therefore, the hot rolling pass experienced in the production method of the present invention becomes more numerous than the pass in the prior rolling process. Less, the hot rolling process step is simpler, the required hot rolling and rolling time is more economical, and the working efficiency is higher.
  • the annealing temperature is 150 to 400 ° C, and the annealing time is 10 to 300 s.
  • the annealing temperature and annealing time also have an extremely important influence on the static recrystallized grain size of the sheet. If the annealing temperature is too high, the rate of static recrystallized grain growth is too fast, so that it is difficult to obtain fine recrystallized grains. If the annealing temperature is too low, the deformation energy storage does not reach the energy required for static recrystallization at this temperature, so that static recrystallization does not occur and the crystal grains cannot be further refined. At the same time, at a certain annealing temperature, as the annealing time increases, the deformed grains will form fine grains by static recrystallization and gradually grow.
  • the annealing temperature should be controlled between 150 and 400 ° C, and the annealing time should be controlled between 10 and 300 s to effectively refine the crystal of the magnesium alloy sheet.
  • the particle size greatly increases the room temperature strength and elongation of the magnesium alloy sheet.
  • the step of preparing the rolled blank in step 1) of the preparation method of the present invention comprises smelting, casting ingot, homogenization treatment, sawing ingot casting and rough rolling.
  • the rolling speed for controlling each pass of the rough rolling is 10 to 50 m/min.
  • the reduction amount of each pass of the rough rolling is controlled to be 10 to 30%.
  • the rolling pass in the step (1) is relatively small, and therefore, the rolling is controlled during the rough rolling.
  • the secondary reduction is 10 to 30%, which is less than the rolling reduction of each pass in the high-efficiency hot rolling process.
  • the billet is preheated before each pass of the rough rolling, and the pre-control is controlled.
  • the rolling temperature of each of the hot temperature and the rough rolling is 250 to 450 °C.
  • the reason why the preheating temperature and the rolling temperature of each pass of the rough rolling are in the range of 250 to 450 ° C is that the temperature is too high, and the crystal grains are rapidly grown at a high temperature before and after rolling, and the temperature is lowered.
  • the effect of refining the grains by rolling deformation if the temperature is too low, the plastic deformation ability of the material is low, and the rolled sheet is easily cracked or even broken.
  • the rolled blank in the step 1) of the preparation method of the present invention, may also be prepared by a two-roll casting method. This method is a conventional process in the art, and therefore will not be described again here.
  • the preparation method of the high-strength and high-ductility magnesium alloy sheet according to the present invention adopts a faster rolling speed and a large rolling reduction, so that the magnesium alloy sheet with high deformation energy storage but no dynamic recrystallization has occurred.
  • Short-time annealing is performed at a subsequent lower annealing temperature to obtain fine crystal grains resulting from static recrystallization in the magnesium alloy sheet material, thereby obtaining a magnesium alloy sheet having higher strength and better plasticity.
  • magnesium alloy sheet with high strength and good plasticity can be obtained by controlling the rolling process parameters and the annealing process parameters, and the process steps are simple and convenient, and the production process is simple and convenient.
  • High efficiency under the premise of improving the mechanical properties of magnesium alloy sheet, it also reduces the production cost of magnesium alloy sheet, which has high practical application value and can be widely extended to related production and manufacturing fields.
  • the high-efficiency rolling process of the high-strength and high-ductility magnesium alloy sheet according to the present invention has a suitable rolling speed and a reduction in the pass reduction, and can be widely extended to related production and manufacturing fields.
  • the high-efficiency rolling process of the high-strength and high-ductility magnesium alloy sheet has a proper rolling pass control, which advantageously improves the rolling efficiency.
  • the high-efficiency rolling process of the high-strength and high-ductility magnesium alloy sheet according to the present invention can effectively improve the mechanical properties of the sheet, and in particular, can greatly improve the strength and ductility of the sheet.
  • the strength and plasticity of the magnesium alloy sheet can be improved by the preparation method of the high strength and high ductility magnesium alloy sheet according to the present invention.
  • the method for preparing the high-strength and high-ductility magnesium alloy sheet has good rollability.
  • the preparation method of the high-strength and high-ductility magnesium alloy sheet can greatly reduce the rolling pass, thereby effectively reducing the time required for production preparation, increasing the production efficiency, and further reducing the production cost.
  • the preparation method of the high-strength and high-ductility magnesium alloy sheet has a simple process step and can be widely extended to relevant production and manufacturing fields.
  • Figure 1 is a microstructure diagram of Comparative Example B1 after an annealing step.
  • Comparative Example B2 is a microstructure diagram of Comparative Example B2 after an annealing step.
  • Figure 3 is a microstructure diagram of Example A1 after an annealing step.
  • Example 4 is a graph showing the relationship between the amount of reduction used in Example A1, Comparative Example B1, and Comparative Example B2 and its room temperature tensile curve.
  • Figure 5 is a microstructure diagram of Comparative Example B3 after an annealing step.
  • Figure 6 is a microstructure diagram of Comparative Example B4 after an annealing step.
  • Figure 7 is a microstructure diagram of Example A2 after an annealing step.
  • Figure 8 is a graph showing the relationship between the amount of reduction used in Example A2, Comparative Example B3, and Comparative Example B4 and its room temperature tensile curve.
  • Figure 9 is a microstructure diagram of Comparative Example B5 after an annealing step.
  • Figure 10 is a microstructure diagram of Comparative Example B6 after an annealing step.
  • Figure 11 is a microstructure diagram of Example A3 after an annealing step.
  • Figure 12 is a graph showing the relationship between the amount of reduction used in Example A3, Comparative Example B5, and Comparative Example B6 and its room temperature tensile curve.
  • (1d) sawing ingot after homogenization treatment, the ingot is sawn into a slab having a thickness of 5 mm according to the thickness requirement;
  • (1e) rough rolling the parameters of the rolling process are controlled as follows: the diameter of the rolls is 75 mm, the rolling speed of each pass is 10 to 50 m/min, and the reduction of each pass is 10 to 30%, each pass Preheating the billet before rolling, the preheating temperature and the rolling temperature are both 250-450 ° C, and the preheating holding time is 1-15 min.
  • the rolled billets of Examples A3 and A6 were obtained by twin-roll casting and obtained AZ31 alloy billets having an initial thickness of 2 mm.
  • the roll diameter is 75mm
  • the rolling speed for controlling each rolling pass is 10 ⁇ 50m/min
  • the rolling reduction of each rolling pass is 40-90%
  • each rolling pass is
  • the billet is preheated before rolling, and the preheating temperature and the rolling temperature are controlled to be 250 to 450 ° C, and the preheating holding time is 1 to 15 min.
  • the controlled annealing temperature is 150 to 400 ° C, and the annealing time is 10 to 300 s.
  • Comparative Examples B5, B6, and B9 were also obtained by twin-roll casting.
  • Comparative Examples B1-B4, B7, B8 were obtained by smelting, casting ingot, homogenization treatment, sawing ingot casting and rough rolling steps.
  • Table 1 lists the specific process parameters of Examples A1-A6 and Comparative Examples B1-B9.
  • the magnesium alloy sheets of Examples A1-A6 and Comparative Examples B1-B9 were sampled, and the middle portion of the sample was taken to observe the microstructure of the sheet.
  • the microstructure of the relevant sheets was as shown in the following figures: Correlation of mechanical properties by conventional tensile test The test method was used for the determination; wherein the tensile strain rate was 10 -3 /s and the gauge length was 10 mm, and the results obtained after the test were shown in Table 2.
  • Table 2 lists the mechanical property parameters of Examples A1-A6 and Comparative Examples B1-B9.
  • the yield strengths of Examples A1 to A6 were both ⁇ 234 MPa, and the tensile strength was ⁇ 255 MPa, indicating that the magnesium alloy sheet of the examples had higher strength; the uniform extension of Examples A1 - A6 The rate ⁇ 8% and the elongation ⁇ 20%, thereby indicating that the magnesium alloy sheet of the example has high ductility and good plasticity.
  • the yield strength, tensile strength, uniform elongation, and elongation of Examples A1 to A6 were both higher than the yield strength, tensile strength, uniform elongation, and elongation of the corresponding comparative examples.
  • the yield strength of the magnesium alloy sheet of the examples was greatly improved, for example, the yield strength (265 MPa) of Example A6 was increased by 35.9% as compared with the yield strength (195 MPa) of Comparative Example B9, as compared with The yield strength of the comparative example B8 (141 MPa), the yield strength of the example A5 (234 MPa) increased by about 66%, and the yield strength of the comparative example B7 (119 MPa). In comparison, the yield strength (245 MPa) of Example A4 was even increased by about 106%.
  • Comparative Example B1 As shown in Fig. 1, if necessary, refer to Table 1.
  • the single pass reduction of Comparative Example B1 is 10%.
  • the deformation of the magnesium alloy sheet is small due to the small amount of reduction, so that the recrystallization of the sheet is incomplete.
  • the recrystallized grain fraction is only 22%, and the crystal grains thereof are relatively coarse, and the average grain size is about 9 ⁇ m.
  • the single pass reduction of Comparative Example B2 is 30%, and the deformation of the magnesium alloy sheet is large due to the large single pass reduction compared to Comparative Example B1.
  • the amount is also relatively large.
  • the recrystallization of the magnesium alloy sheet is still incomplete, the recrystallized grain fraction is higher than that of the comparative B1, and the recrystallized grain fraction is about 40%.
  • the particle size is smaller, which is about 6 ⁇ m.
  • Example A1 As shown in Figure 3, if necessary, see Table 1.
  • the single pass reduction of Example A1 is 50%, because the single pass reduction is larger than that of Comparative Examples B1 and B2.
  • the deformation of the alloy sheet is larger, the grain structure of the magnesium alloy sheet is remarkably refined, and the large-sized deformed grains are greatly reduced.
  • the grain size of Example A1 shown in FIG. 3 is smaller, the grain size is more uniform, and the average grain size is larger. At about 4 ⁇ m, the recrystallized grain fraction reached about 68%.
  • Comparative Example B1 and Comparative Example B2 employ relatively low single pass reductions, so Comparative Example B1 and Comparative Example B2
  • the recrystallized grain size in the microstructure presented after the annealing step is large, and the recrystallized grain refining effect is not obvious.
  • FIG. 3 and in conjunction with the contents shown in Table 1, it is known that since Example A1 employs a relatively high single-pass reduction, the degree of recrystallization in the microstructure of Example A1 is very remarkable, and the crystal grains are very remarkable. Small size and uniform grain size.
  • Figure 4 shows the relationship between the single pass reduction used in Example A1, Comparative Example B1 and Comparative Example B2 and its room temperature tensile curve.
  • the single pass reduction of Comparative Example B1 was 10%, and the single pass reduction of Comparative Example B2 was 30%, and Example A1 used The single pass reduction is 50%.
  • the mechanical properties of the magnesium alloy sheet increase. Specifically, the yield strength, tensile strength, uniform elongation, and elongation of Example A1 were higher than Comparative Example B1.
  • Figures 5, 6, and 7 show the microstructures of Comparative Example B3, Comparative Example B4, and Example A2 after the annealing step, respectively.
  • Comparative Example B3 As shown in Fig. 5, if necessary, refer to Table 1.
  • the single pass reduction of Comparative Example B3 is 10%.
  • the deformation of the magnesium alloy sheet is small due to the small amount of reduction, so that the recrystallization of the sheet is incomplete.
  • the recrystallized grain fraction is only 30%, and the crystal grains seen from Fig. 5 are coarser, and the average grain size is about 7 ⁇ m.
  • Comparative Example B4 As shown in Fig. 6, if necessary, see Table 1.
  • the single pass reduction of Comparative Example B4 is 30%, which is larger than the single pass reduction used in Comparative Example B3.
  • the deformation of the sheet is larger.
  • the recrystallized grain fraction is higher than that of the comparative B3, and the recrystallized grain fraction is about 48%.
  • the grain size is smaller, which is about 4 ⁇ m.
  • Example A2 uses a single pass reduction of 50%, due to the larger single pass reduction compared to Comparative B3 and B4, magnesium alloy
  • the deformation of the sheet is larger, the grain structure of the magnesium alloy sheet is remarkably refined, and the large-sized deformed grains are greatly reduced.
  • the grain size of the embodiment A2 shown in Fig. 7 is finer, the grain size is more uniform, and the average crystal size.
  • the particle size is about 3 ⁇ m, and the recrystallized grain fraction reaches about 66%.
  • Comparative Example B3 and Comparative Example B4 were The recrystallized grain size in the microstructure presented after the annealing step is relatively large, and the recrystallized grain refining effect is not obvious.
  • FIG. 7 and in conjunction with the contents shown in Table 1 since Example A2 employs a higher single pass reduction, the recrystallization effect in the microstructure of Example A2 is remarkable, and the grain size is as follows. Small and uniform in grain size.
  • Figure 8 shows the relationship between the single pass reduction used in Example A2, Comparative Example B3 and Comparative Example B4 and its room temperature tensile curve.
  • the single pass reduction of Comparative Example B3 was 10%, and the single pass reduction of Comparative Example B4 was 30%, while Example A2 used
  • the single pass reduction is 50%.
  • the stress and strain index of the magnesium alloy sheet also increases. Specifically, the yield strength, tensile strength, uniform elongation, and elongation of Example 2 were higher than the comparative examples. Yield strength, tensile strength, uniform elongation, and elongation of B3 and B4.
  • Comparative Example B5 As shown in Fig. 9, if necessary, refer to Table 1.
  • the single pass reduction of Comparative Example B5 is 10%.
  • the deformation of the magnesium alloy sheet is small due to the small amount of reduction, so that the recrystallization of the sheet is incomplete.
  • the recrystallized grain fraction is only 28%, and the crystal grains seen from Fig. 9 are coarser and the average grain size is about 12 ⁇ m.
  • Comparative Example B6 As shown in Fig. 10, if necessary, see Table 1.
  • the single pass reduction of Comparative Example B6 is 30%, which is larger than the single pass reduction used in Comparative Example B5.
  • the deformation of the sheet is larger.
  • the recrystallized grain fraction is higher than that of the comparative B5, and the recrystallized grain fraction is about 48%.
  • the grain size is smaller, which is about 7 ⁇ m.
  • Example A3 uses a single pass reduction of 50%, due to the larger single pass reduction compared to Comparative B5 and B6, magnesium alloy
  • the deformation of the sheet is larger, the grain structure of the magnesium alloy sheet is remarkably refined, and the large-sized deformed grains are greatly reduced.
  • the grain size of Example A3 shown in Fig. 11 is finer, the grain size is more uniform, and the average crystal size.
  • the particle size is about 4 ⁇ m, and the recrystallized grain fraction reaches about 67%.
  • Comparative Example B5 and Comparative Example B6 were The recrystallized grain size in the microstructure presented after the annealing step is large, and the recrystallized grain refining effect is not obvious. As shown in FIG. 11 and in conjunction with the contents shown in Table 1, since Example A3 employs a higher single pass reduction, the recrystallization effect in the microstructure of Example A3 is remarkable, and the grain size is as follows. Small and uniform in grain size.
  • Figure 12 shows the relationship between the single pass reduction used in Example A3, Comparative Example B5 and Comparative Example B6 and its room temperature tensile curve.
  • the single pass reduction of Comparative Example B5 was 10%, and the single pass reduction of Comparative Example B6 was 30%, while Example A3 used
  • the single pass reduction is 50%.
  • the stress and strain index of the magnesium alloy sheet also increases. Specifically, the yield strength, tensile strength, uniform elongation, and elongation of Example A3 were higher than the comparison. Yield strength, tensile strength, uniform elongation, and elongation of Examples B5 and B6.

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Abstract

一种镁合金板材的高效率轧制工艺，其为对轧制坯料进行轧制的工艺，该轧制工艺的参数为：各轧制道次的轧制速度为10-50m/min，各轧制道次的压下量控制在40-90％，各轧制道次轧制前的预热温度和轧制温度均为250-450℃。一种镁合金板材的制备方法，其包括步骤：1)制备轧制坯料；2)高效热轧：控制各轧制道次的轧制速度为10-50m/min，各轧制道次的压下量为40-90％，各轧制道次轧制前的预热温度和轧制温度均为250-450℃；3)退火。所述轧制工艺后还能有效地改善板材的力学性能水平，尤其是能够大幅度提高板材的强度和延展性。

Description

[根据细则37.2由ISA制定的发明名称]　镁合金板材的轧制及制备方法 技术领域
本发明涉及一种有色金属加工工艺，尤其涉及一种用于镁合金板材的轧制工艺。
背景技术
镁是迄今为止发现的最轻金属结构材料，为此，镁合金作为一种新兴的金属结构材料，在世界范围内有着丰富的资源。镁的密度仅为1.74g/cm3，其仅为铝密度的2/3，钢密度的1/4。这一特性使得镁合金在汽车、航空航天、国防军事、电子通信、家电领域有着非常广泛的应用前景。轧制作为一种金属材料塑性变形加工的重要手段得到了长足的发展。然而，现有的镁合金板材的应用仍然受到很大的限制，其生产量和使用量远不及钢铁和其他有色金属(例如铝和铜)。如何克服各种制约因素将其广泛地推广至相关领域用于生产制造是镁合金进一步发展所要面临的重大课题。
制约镁合金板材的发展的因素主要有以下几点：首先，镁合金属于密排六方晶体结构，独立滑移系少，室温加工性能较差，因此，现有技术中的镁合金板材的生产制造均采用多道次且小压下量的方式在高温下(热轧)进行，在现有的常规工序生产中轧制镁合金中厚板就要多达十余道次。其次，轧制镁合金板材的单道次压下量一般较小(单道次压下量通常小于30％)，其远远小于钢铁及铝、铜等有色金属的单道次压下量，由此使得轧制工序多、生产成本高、生产效率低下。再者，一般认为镁合金的塑性会随着应变速率的提高而下降，因此轧制时通常采用的轧制速度(轧制速度通常小于5m/min)，其也远远小于钢铁及铝、铜等有色金属，因此也会提高镁合金板材的生产成本，并降低镁合金板材的生产效率。最后，镁合金板材的力学性能较差，尤其是需要进一步地改进镁合金板材的强度和延展性。
公开号为CN101648210A，公开日为2010年2月17日，名称为“低温高速大加工量轧制变形镁合金板材的加工方法”的中国专利文献公开了一种用于 镁合金板材的加工方法。该加工方法包括步骤如下：在传统的铸锭(扁坯)→铣面(铣边)→探伤→均匀化处理→加热→热轧→矫直→锯切→表面处理→检测→涂油包装的扁锭加热-热轧生产中厚板的工艺基础上，针对工艺中的热轧工艺采用控制轧制温度、轧制速度(尤其是终轧温度及速度)及每道次的压下量、道次控制在8～10之间，各道次变形之间的间隔时间以及冷却速度的方法来控制镁合金热轧板的晶粒度达到提高其综合力学性能的目的。然而，该加工方法的工艺步骤较为复杂，并且轧制速度高达180m/min，使得其很难广泛地应用于实际生产中。同时，轧制单道次加工率最大时也仅为30～42％，单道次压下量较小，道次加工效率并不高。
此外，公开号为CN103316915A，公开日为2013年9月25日，名称为“一种宽幅镁合金板材的制备方法”的中国专利文献公开了一种宽幅镁合金板材高效制备方法。该制备方法的步骤包括：将细晶、均质、低内应力的镁合金板坯经均匀化处理后进行可逆高速热轧，在可逆高速热轧过程中多次采用中间道次高温预退火以及与立辊轧制和预拉伸相结合的方式对板材进行超大压下变形，经过数道次热轧后即可获得镁合金中厚度板，利用上述方法获得中厚板经切头尾和剪边处理后，对表面进行打磨抛光处理后，经加热退火后精轧，在精轧程过中多次采用中间道次高温预退火以及与反复弯曲变形和高速异步轧制相结合对板材进行超大压下变形，获得高精度的镁合金板材。然而，该中国专利文献所公开的加工方法中的轧制速度过快，存在着一定的安全隐患。与此同时，该加工方法的工艺步骤较为复杂，也很难广泛地应用于实际生产中。
综上所述，现有的镁合金板材制备方法并不能有效地兼顾提高生产效率、降低生产成本及改善力学性能等诸多方面。同时，由于现有的镁合金板材制备方法要么轧制速度过高，要么轧制速度过低，并且工序复杂，因此其并不具有大规模工业化生产的可行性。为此，企业亟需获得一种轧制加工工艺，其能够满足市场对于镁合金板材应用需求的增长。
发明内容
本发明的目的在于提供一种高强度高延展性镁合金板材的高效率轧制工艺。该轧制工艺的轧制速度及道次压下量适当，能够广泛地推广至相关生产制造领域。另外，该轧制工艺的轧制总道次控制得当，有利地提高了轧制效率。 此外，采用本发明所述的轧制工艺后还能有效地改善板材的力学性能水平，尤其是能够大幅度地提高板材的强度和延展性。
为了实现上述目的，本发明提出了一种高强度高延展性镁合金板材的高效率轧制工艺，其为对轧制坯料进行轧制的工艺，该轧制工艺的参数控制为：各轧制道次的轧制速度为10～50m/min，各轧制道次的压下量控制在40～90％，在各轧制道次轧制前预热坯料，并控制各轧制道次轧制前的预热温度和轧制温度均为250-450℃。
需要说明的是，在本技术方案中，各轧制道次的压下量在上述范围内可以相同，也可以不同。
镁合金材料通过晶粒细化可以获得更为优良的力学性能，也就是说，通过晶粒细化不仅能提高镁合金材料的加工塑性，而且还能提高镁合金材料的强度，并降低其力学性能的各向异性。相较于铁、铝等其它合金材料，因为镁合金材料具有更大的Hall-Petch关系的K系数，所以晶粒细化作用对于提高镁合金材料的强度的贡献更加明显。为了进一步提高镁合金的强度和韧度及其它力学性能，就需要得到更加细小的晶粒组织。在挤压、轧制、锻造等变形加工过程中，铸态组织中粗大晶粒和粗大的第二相逐渐得到破碎细化，使得第二相弥散分布于镁基体中，从而令镁合金的力学性能得到进一步地提高，进而获得更高的强度和更好的塑性。
经轧制后的镁合金板材的组织特征，如晶粒尺寸、织构等与轧制工艺中的轧制速度、单道次压下量(尤其是终轧压下量)、轧制温度、退火温度和退火时间都有着密切的关系。一方面，当镁合金材料轧制速度较快时，变形所产生的变形热以及轧件与轧辊接触所产生的摩擦热会导致轧件实际温度的上升，启动更多的变形模式，以提高合金的变形能力，从而在镁合金板材的微观组织中引入更多的位错，诱发动态再结晶，细化变形晶粒，进而获得组织晶粒更为细小的镁合金板材。另一方面，提高轧制变形应变量也有利于轧制变形过程中获得更加细化的微观组织。变形是促使板材发生再结晶驱动力的来源。与此同时，压下量又决定了变形程度和变形储能大小，从而影响静态再结晶的形核速率，进而最终决定静态再结晶晶粒的尺寸大小。较大的变形量能够在镁合金的组织中引入更多的畸变能量，以降低动态再结晶的起始温度，以此更加有利于镁合金板材中获得更加细化的组织结构。鉴于此，采用较快轧制速度与较大的轧制 压下量相结合的轧制工艺，不仅能够有效地获得细晶组织，以提高镁合金板材的力学性能，而且还能够有利地提高轧制的工作效率。
基于本发明的技术方案，采用适当较高的轧制速度并且匹配较大的轧制变形量，有望在镁合金板材中获得细小的变形组织。对轧制镁合金板材来说，轧制速度主要会影响其变形速率。变形速率对轧制速度的影响主要表现在两方面：一方面是变形速率将影响变形过程中轧件的实际轧制温度；另一方面是变形速率会影响轧制过程中可启动的变形模式。这两个方面将综合性地决定特定轧制温度下轧件的最终可轧制能力。发明人发现，在实际生产过程中，当轧制速度为12.1m/min时，在适当的轧制温度下单道次压下量可以达到60％，并且伴随着动态再结晶的发生，为此，提高轧制速度既可以有效地改善镁合金板材的轧制能力，也实现了较大压下量轧制的应用。然而，如果轧制速度过快，变形所产生的变形热以及轧件与轧辊接触所产生的摩擦热会导致轧件实际温度的大幅度上升，由于轧件的轧制温度(即动态再结晶温度)在实际生产过程中很难控制，从而会诱发动态再结晶并可使晶粒长大，使得镁合金板材组织再结晶不完全或者再结晶晶粒相对粗大，进而导致镁合金板材的最终力学性能较差。为此，轧制速度不宜超过50m/min。但是，如果轧制速度过慢，变形所产生的变形热和轧件与轧辊接触所产生的摩擦热又不足以引起轧件实际温度的提高，反而会因预热轧件与常温轧辊的接触而失去了轧件的部分热量，由此慢速轧制也不能实现较大压下量的轧制。由于压下量小会使得变形储能和位错密度降低，在静态再结晶过程中，不具有充足的形核驱动力，不利于细化晶粒，会影响镁合金板材的强度提高。鉴于此，需要将各轧制道次的轧制速度控制在10～50m/min范围之间。
另外，提高轧制压下量有利于增加板材中储存的变形能，使得镁合金板材中具有较高的位错密度，为静态再结晶形核提供更大的驱动力，从而可以有效地细化晶粒，提高板材的强度和延展性。发明人还发现，各道次的压下量对镁合金板材的微观组织有着重要的影响。随着压下量的增大，镁合金板材的晶粒内位错密度增加，晶格畸变加剧，再结晶晶粒形核数目增多，由此使得板材内的晶粒得以大幅度地细化。但是，若单道次压下量过大，也会导致轧件开裂的可能倾向显著增加，故而单道次压下量不宜大于90％。相反，若单道次压下量过小，则变形储能和位错密度低，在静态再结晶过程中，形核不具有充足的驱 动力，形核点少，不利于镁合金板材的晶粒细化。因此，在本发明所述的高强度高延展性镁合金板材的高效率轧制工艺中的各轧制道次的单道次压下量不得小于40％且不得大于90％。
由于上述技术方案中的各轧制道次的压下量控制在40～90％之间，每一道次的压下量变得更大了，因此，相较于现有的轧制工序中所需的道次，本发明所述的轧制工艺中所经历的轧制道次更少，工序步骤更为简单，所需的轧制时间更省，工作效率更高。
此外，在通过控制轧制速度及轧制单道次压下量的基础上，控制轧制温度能够有效地改善镁合金板材的力学性能。在本发明的技术方案中，将各轧制道次的轧制前的预热温度和轧制温度都控制在250～450℃之间的原因在于：温度过高，轧制前后晶粒在高温下快速长大，降低了通过轧制变形来细化晶粒的效果；如温度过低，则材料的塑性变形能力较低，轧制板材容易开裂、甚至原料发生断裂。
进一步地，在本发明所述的高强度高延展性镁合金板材的高效率轧制工艺中，控制各轧制道次轧制前的预热时间为1～15min。
本发明的另一目的在于提供一种高强度高延展性镁合金板材的制备方法。通过该制备方法可以获得强度高且延展性好的镁合金板材。另外，该制备方法的工序步骤简单，所耗时间少，生产效率高。此外，本发明所述的高强度高延展性镁合金板材的制备方法的生产成本低，能够大规模地推广至相关生产制造领域。
为了达到上述发明目的，本发明提出了一种高强度高延展性镁合金板材的制备方法，其包括步骤：
(1)制备轧制坯料；
(2)将坯料高效热轧到目标值：各轧制道次的轧制速度为10-50m/min，各轧制道次的压下量控制在40-90％，在各轧制道次轧制前预热坯料，并控制各轧制道次轧制前的预热温度和轧制温度均为250-450℃；
(3)退火。
进一步地，在本发明所述的制备方法中，在步骤(2)中，控制各轧制道次轧制前的预热时间为1～15min。
通过控制在高效热轧过程中的轧制速度、轧制单道次压下量和轧制温度不 仅能够有效地改善镁合金板材的力学性能，而且能够有利地提高镁合金板材的轧制效率。由于上文已经对于控制轧制工艺参数的设计原理进行了详细的描述，在此，就不再针对上述热轧工艺的参数控制的设计原理进行赘述了。
需要说明的是，由于高效热轧中的各轧制道次的压下量控制在40～90％之间，也就是说，较之于现有技术中所采用的轧制的压下量，每一道次的压下量变得更大了，因此，相较于现有的轧制工序中的道次，本发明所述的制备方法中所经历的热轧轧制道次就会变得更少，热轧工序步骤更为简单，所需的热轧轧制时间更省，工作效率则更高。
进一步地，在上述步骤(3)中，退火温度为150～400℃，退火时间为10～300s。
退火温度和退火时间对板材的静态再结晶晶粒大小也有着极为重要的影响。如果退火温度太高，静态再结晶晶粒长大速率过快，故而很难得到细小的再结晶晶粒。如果退火温度太低，那么变形储能则达不到该温度下静态再结晶所需的能量，故而不会产生静态再结晶，无法进一步地细化晶粒。同时，在一定退火温度下，随着退火时间的增加，变形晶粒将通过静态再结晶形成细小的晶粒并且逐渐长大。同时，一旦保温时间过长，又将导致再结晶晶粒变得粗大，由此不利于提高镁合金板材的强度。反之，保温时间过短，则有可能尚未发生静态再结晶，也无法通过再结晶进一步细化晶粒。为此，根据镁合金板材的成分和变形情况，退火温度应当控制在150～400℃范围之间，并将退火时间应控制在10～300s范围之间，以有效地细化镁合金板材的晶粒尺寸，从而大幅度地提高镁合金板材的室温强度与延伸率。
在某些实施方式中，本发明所述的制备方法的步骤1)制备轧制坯料的步骤包括熔炼、铸造铸锭、均匀化处理、锯切铸锭和粗轧。
更进一步地，在上述步骤(1)中，控制粗轧各道次的轧制速度为10～50m/min。
更进一步地，在上述步骤(1)中，控制粗轧各道次的压下量为10～30％。
考虑扁锭咬入板材的条件，较之于步骤(2)，在步骤(1)中的各轧制道次采用相对较小的轧制压下量，因此，在粗轧过程中控制各道次的压下量为10～30％，其小于高效热轧过程中的各道次的轧制压下量。
更进一步地，在上述步骤(1)中，在粗轧各道次前预热坯料，并控制预 热温度和粗轧各道次的轧制温度为250～450℃。
在步骤(1)中，控制预热温度和粗轧各道次的轧制温度在250～450℃范围之间的原因在于：温度过高，轧制前后晶粒在高温下快速长大，减低了通过轧制变形来细化晶粒的效果；如温度过低，则材料的塑性变形能力较低，轧制板材容易开裂、甚至材料发生断裂。
在另外一些实施方式中，本发明所述的制备方法的步骤1)中，还可以采用双辊铸轧方法制备轧制坯料。该方法为本领域内的常规工艺，故在此不再进行赘述。
本发明所述的高强度高延展性镁合金板材的制备方法采用了较快的轧制速度及较大的轧制压下量，使得变形储能高但尚未发生动态再结晶的镁合金板材，在随后的较低的退火温度下进行短时间退火，以在镁合金板材中获得由静态再结晶导致的细小晶粒，从而得到强度更高且塑性更好的镁合金板材。
此外，在该高强度高延展性镁合金板材的制备方法中，仅需要对于轧制工艺参数和退火工艺参数进行控制即可获得具有强度高且塑性好的镁合金板材，工艺步骤简单便捷，生产效率高，在提高镁合金板材的力学性能指标的前提下，还降低了镁合金板材的生产成本，其具有较高的实际应用价值，可以广泛地推广至相关生产制造领域。
本发明所述的高强度高延展性镁合金板材的高效率轧制工艺的轧制速度和道次压下量适当，能够广泛地推广至相关生产制造领域。
另外，该高强度高延展性镁合金板材的高效率轧制工艺的轧制总道次控制得当，有利地提高了轧制效率。
此外，采用本发明所述的高强度高延展性镁合金板材的高效率轧制工艺后还能有效地改善板材的力学性能指标，尤其是能够大幅度地提高板材的强度和延展性。
通过本发明所述的高强度高延展性镁合金板材的制备方法可以改善镁合金板材的强度和塑性。
另外，该高强度高延展性镁合金板材的制备方法的可轧性好。
此外，该高强度高延展性镁合金板材的制备方法可以大幅度地减少轧制道次，从而有效地减少生产制备所需的时间，提高生产效率高，进而降低生产成本。
同时，该高强度高延展性镁合金板材的制备方法的工序步骤简单，能够大规模地推广至相关生产制造领域。
附图说明
图1为对比例B1经退火步骤后的微观组织图。
图2为对比例B2经退火步骤后的微观组织图。
图3为实施例A1经退火步骤后的微观组织图。
图4为实施例A1、对比例B1和对比例B2所采用的压下量和其室温拉伸曲线的关系图。
图5为对比例B3经退火步骤后的微观组织图。
图6为对比例B4经退火步骤后的微观组织图。
图7为实施例A2经退火步骤后的微观组织图。
图8为实施例A2、对比例B3和对比例B4所采用的压下量和其室温拉伸曲线的关系图。
图9为对比例B5经退火步骤后的微观组织图。
图10为对比例B6经退火步骤后的微观组织图。
图11为实施例A3经退火步骤后的微观组织图。
图12为实施例A3、对比例B5和对比例B6所采用的压下量和其室温拉伸曲线的关系图。
具体实施方式
下面将结合附图说明和具体的实施例对本发明所述的高强度高延展性镁合金板材的高效率轧制工艺及高强度高延展性镁合金板材的制备方法做进一步的解释和说明，然而该解释和说明并不对本发明的技术方案构成不当限定。
实施例A1-A6和对比例B1-B9
通过本发明的高强度高延展性镁合金板材的制备方法来获得上述实施例A1-A6，其包括步骤：
(1)制备轧制坯料：
其中，实施例A1-A2，A4，A5中轧制坯料的制备工艺如下：
(1a)熔炼：将原材料放置在钢坩埚中混合，随后将坩埚及原材料放置在感应炉中加热至760℃熔炼，在熔炼过程中，向感应炉中注入氩气作为保护气氛，防止燃烧；
(1b)铸造铸锭：熔炼完毕后，将熔融的镁合金液体浇铸于200℃的预热钢模具中，铸锭尺寸为55mm(长)*30mm(宽)*120mm(高)；
(1c)均匀化处理：先在300℃温度下均匀化处理12hr，然后在430℃的温度下均匀化处理4hr；
(1d)锯切铸锭：均匀化处理后根据厚度要求将铸锭锯切成5mm厚度的板坯；
(1e)粗轧：该轧制工艺的参数控制为：轧辊直径为75mm，各道次的轧制速度为10～50m/min，各道次的压下量为10～30％，各道次轧制前预热坯料，预热温度和轧制温度均为250～450℃，预热保温时间为1～15min。
实施例A3、A6的轧制坯料通过双辊铸轧制备的得到的AZ31合金坯料，其初始厚度为2mm。
(2)高效热轧：轧辊直径为75mm，控制各轧制道次的轧制速度为10～50m/min，各轧制道次的压下量为40～90％，各轧制道次在轧制前预热坯料，控制预热温度和和轧制的温度为250～450℃，预热保温时间为1～15min。
(3)退火：控制退火温度为150～400℃，退火时间为10～300s。
需要说明的是，对比例B5、B6、B9的轧制坯料也是通过双辊铸轧制备的得到的。而对比例B1-B4，B7，B8是通过熔炼、铸造铸锭、均匀化处理、锯切铸锭和粗轧步骤获得的。
表1列出了实施例A1-A6和对比例B1-B9的具体工艺参数。
表1.
Figure PCTCN2016108674-appb-000001
Figure PCTCN2016108674-appb-000002
Figure PCTCN2016108674-appb-000003
*注：对于表中的多道次轧制，如果单道次压下量只有一个值，则表示每一个道次的压下量均是相同的。
对实施例A1-A6和对比例B1-B9的镁合金板材取样，截取样品中间部分以观察板材的微观组织，相关板材的微观组织如以下附图所示：相关力学性能通过常规的拉伸实验测试方法来测定；其中，拉伸应变速率为10-3/s，标距长度10mm，将经过测试后所获得的结果列于表2中。
表2列出了实施例A1-A6和对比例B1-B9的力学性能参数。
表2.
序号* 屈服强度(MPa) 抗拉强度(MPa) 均匀延伸率(％) 延伸率(％)
A1 243 300 13 24
A2 244 265 8 29
A3 263 304 10 20
A4 245 308 20 26
A5 234 255 16 31
A6 265 318 15 24
B1 221 270 9 15
B2 235 280 11 20
B3 215 236 7 14
B4 238 259 7 18
B5 255 291 8 16
B6 261 303 8 13
B7 119 230 15 23
B8 141 212 9 30
B9 195 264 12 22
从表2所示的内容可以看出，实施例A1-A6的屈服强度均≥234MPa，抗拉强度≥255MPa，说明实施例的镁合金板材具有较高的强度；实施例A1-A6的均匀延伸率≥8％且延伸率≥20％，由此说明实施例的镁合金板材具有较高的延展性，具备良好的塑性。实施例A1-A6的屈服强度、抗拉强度、均匀延伸率、延伸率均高于其所对应的对比例的屈服强度、抗拉强度、均匀延伸率、延伸率。尤其是，实施例的镁合金板材的屈服强度得到大幅度地提高，例如，较之于对比例B9的屈服强度(195MPa)，实施例A6的屈服强度(265MPa)提高了35.9％，相较于对比例B8的屈服强度(141MPa)，实施例A5的屈服强度(234MPa)的升幅达到了66％左右，与对比例B7的屈服强度(119MPa) 相比较，实施例A4的屈服强度(245MPa)甚至提升了约106％。
图1、图2和图3分别显示了对比例B1、对比例B2和实施例A1经退火步骤后的微观组织。
如图1所示，必要时可以参见表1，对比例B1的单道次压下量为10％，由于压下量小导致镁合金板材的变形量小，因此，使得板材的再结晶不完全，其再结晶晶粒分数仅为22％，并且其晶粒比较粗大，平均晶粒尺寸在9μm左右。
如图2所示，必要时可以参见表1，对比例B2的单道次压下量为30％，由于较之于对比例B1所采用的单道次压下量大，镁合金板材的变形量也相对较大，尽管镁合金板材的再结晶仍不完全，但是其再结晶晶粒分数要高于对比例B1的再结晶晶粒分数，其再结晶晶粒分数为40％左右，平均晶粒尺寸更小，其约为6μm。
如图3所示，必要时可以参见表1，实施例A1采用的单道次压下量为50％，由于较之于对比例B1和B2所采用的单道次压下量更大，镁合金板材的变形量更大，镁合金板材的晶粒组织明显得到细化，大尺寸变形晶粒大幅度地减少。较之于图1和图2所示的对比例B1和B2的镁合金板材的晶粒尺寸，图3所示的实施例A1的晶粒尺寸更小，晶粒大小较为均匀，平均晶粒尺寸在4μm左右，再结晶晶粒分数达到了68％左右。
如图1和图2所示，并结合表1所示内容可以获知，由于对比例B1和对比例B2采用了相对较低的单道次压下量，因此，对比例B1和对比例B2经退火步骤后所呈现的微观组织中的再结晶晶粒尺寸较大，再结晶细化晶粒效果并不明显。如图3所示，并结合表1所示内容可以获知，由于实施例A1采用了较高的单道次压下量，因此，实施例A1的微观组织中的再结晶程度非常明显，晶粒尺寸小且晶粒大小均匀。
图4显示了实施例A1、对比例B1和对比例B2所采用的单道次压下量和其室温拉伸曲线之间的关系。
如图4所示，并结合表1和表2，对比例B1采用的单道次压下量为10％，对比例B2采用的单道次压下量为30％，而实施例A1采用的单道次压下量为50％，随着单道次压下量的增大，镁合金板材的力学性能指标随之提升。具体地，实施例A1的屈服强度、抗拉强度、均匀延伸率、延伸率均高于对比例B1 和B2的屈服强度、抗拉强度、均匀延伸率、延伸率。
图5、图6和图7分别显示了对比例B3、对比例B4和实施例A2经退火步骤后的微观组织。
如图5所示，必要时可以参见表1，对比例B3的单道次压下量为10％，由于压下量小导致镁合金板材的变形量小，因此，使得板材的再结晶不完全，其再结晶晶粒分数仅为30％，并且从图5中看到的晶粒较为粗大，平均晶粒尺寸在7μm左右。
如图6所示，必要时可以参见表1，对比例B4的单道次压下量为30％，由于较之于对比例B3所采用的单道次压下量要来的大，镁合金板材的变形量更大，虽然镁合金板材的再结晶仍不完全，但是其再结晶晶粒分数要高于对比例B3的再结晶晶粒分数，其再结晶晶粒分数为48％左右，平均晶粒尺寸更小，其约为4μm。
如图7所示，必要时可以参见表1，实施例A2采用单道次压下量为50％，由于较之于对比例B3和B4所采用的单道次压下量更大，镁合金板材的变形量更大，镁合金板材的晶粒组织明显得到细化，大尺寸变形晶粒大幅度地减少。较之于图5和图6所示的对比例B3和B4的镁合金板材的晶粒尺寸，图7所示的实施例A2的晶粒尺寸更加地细小，晶粒大小更为均匀，平均晶粒尺寸在3μm左右，再结晶晶粒分数达到了66％左右。
如图5和图6所示，并结合表1所示内容可以获知，由于对比例B3和对比例B4采用了相对较低的单道次压下量，因此，对比例B3和对比例B4经退火步骤后所呈现的微观组织中的再结晶晶粒尺寸相对较大，再结晶细化晶粒效果并不明显。如图7所示，并结合表1所示内容可以获知，由于实施例A2采用了较高的单道次压下量，因此，实施例A2的微观组织中的再结晶效果明显，晶粒尺寸小且晶粒大小均匀。
图8显示了实施例A2、对比例B3和对比例B4所采用的单道次压下量和其室温拉伸曲线之间的关系。
如图8所示，并结合表1和表2，对比例B3采用的单道次压下量为10％，对比例B4采用的单道次压下量为30％，而实施例A2采用的单道次压下量为50％，随着单道次压下量的增大，镁合金板材的应力和应变指数也随之提升。具体地，实施例2的屈服强度、抗拉强度、均匀延伸率、延伸率均高于对比例 B3和B4的屈服强度、抗拉强度、均匀延伸率、延伸率。
图9、图10和图11分别显示了对比例B5、对比例B6和实施例A3经退火步骤后的微观组织。
如图9所示，必要时可以参见表1，对比例B5的单道次压下量为10％，由于压下量小导致镁合金板材的变形量小，因此，使得板材的再结晶不完全，其再结晶晶粒分数仅为28％，并且从图9中看到的晶粒较为粗大，平均晶粒尺寸在12μm左右。
如图10所示，必要时可以参见表1，对比例B6的单道次压下量为30％，由于较之于对比例B5所采用的单道次压下量要来的大，镁合金板材的变形量更大，虽然镁合金板材的再结晶仍不完全，但是其再结晶晶粒分数要高于对比例B5的再结晶晶粒分数，其再结晶晶粒分数为48％左右，平均晶粒尺寸更小，其约为7μm。
如图11所示，必要时可以参见表1，实施例A3采用单道次压下量为50％，由于较之于对比例B5和B6所采用的单道次压下量更大，镁合金板材的变形量更大，镁合金板材的晶粒组织明显得到细化，大尺寸变形晶粒大幅度地减少。较之于图9和图10所示的对比例B5和B6的镁合金板材的晶粒尺寸，图11所示的实施例A3的晶粒尺寸更加地细小，晶粒大小更为均匀，平均晶粒尺寸在4μm左右，再结晶晶粒分数达到了67％左右。
如图9和图10所示，并结合表1所示内容可以获知，由于对比例B5和对比例B6采用了相对较低的单道次压下量，因此，对比例B5和对比例B6经退火步骤后所呈现的微观组织中的再结晶晶粒尺寸较大，再结晶细化晶粒效果并不明显。如图11所示，并结合表1所示内容可以获知，由于实施例A3采用了较高的单道次压下量，因此，实施例A3的微观组织中的再结晶效果明显，晶粒尺寸小且晶粒大小均匀。
图12显示了实施例A3、对比例B5和对比例B6所采用的单道次压下量和其室温拉伸曲线之间的关系。
如图12所示，并结合表1和表2，对比例B5采用的单道次压下量为10％，对比例B6采用的单道次压下量为30％，而实施例A3采用的单道次压下量为50％，随着单道次压下量的增大，镁合金板材的应力和应变指数也随之提升。具体地，实施例A3的屈服强度、抗拉强度、均匀延伸率、延伸率均高于对比 例B5和B6的屈服强度、抗拉强度、均匀延伸率、延伸率。
需要注意的是，以上列举的仅为本发明的具体实施例，显然本发明不限于以上实施例，随之有着许多的类似变化。本领域的技术人员如果从本发明公开的内容直接导出或联想到的所有变形，均应属于本发明的保护范围。

Claims (10)

  1. 一种高强度高延展性镁合金板材的高效率轧制工艺，其为对轧制坯料进行轧制的工艺，其特征在于，该轧制工艺的参数控制为：各轧制道次的轧制速度为10-50m/min，各轧制道次的压下量控制在40-90％，在各轧制道次轧制前预热坯料，并控制各轧制道次轧制前的预热温度和轧制温度均为250-450℃。
  2. 如权利要求1所述的高强度高延展性镁合金板材的高效率轧制工艺，其特征在于，控制各轧制道次轧制前的预热时间为1～15min。
  3. 一种高强度高延展性镁合金板材的制备方法，其特征在于，包括步骤：
    1)制备轧制坯料；
    2)将坯料高效热轧到目标值：各轧制道次的轧制速度为10-50m/min，各轧制道次的压下量控制在40-90％，在各轧制道次轧制前预热坯料，并控制各轧制道次轧制前的预热温度和轧制温度均为250-450℃；
    3)退火。
  4. 如权利要求3所述的制备方法，其特征在于，在步骤2)中，控制各轧制道次轧制前的预热时间为1～15min。
  5. 如权利要求3或4所述的制备方法，其特征在于，在步骤3)中，退火温度为150-400℃，退火时间为10-300s。
  6. 如权利要求3或4所述的制备方法，其特征在于，在所述步骤1)中制备轧制坯料的步骤包括熔炼、铸造铸锭、均匀化处理、锯切铸锭和粗轧。
  7. 如权利要求6所述的制备方法，其特征在于，在所述步骤1)中，控制粗轧各道次的轧制速度为10-50m/min。
  8. 如权利要求6所述的制备方法，其特征在于，在所述步骤1)中，控制粗轧各道次的压下量为10-30％。
  9. 如权利要求6所述的制备方法，其特征在于，在所述步骤1)中，在粗轧各道次前预热坯料，并控制预热温度和粗轧各道次的轧制温度为250～450℃。
  10. 如权利要求3或4所述的制备方法，其特征在于，在所述步骤1)中，采 用双辊铸轧方法制备轧制坯料。
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