WO2022147922A1 - 梯度纳米结构金属材料及其制备方法 - Google Patents

梯度纳米结构金属材料及其制备方法 Download PDF

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Publication number
WO2022147922A1
WO2022147922A1 PCT/CN2021/085661 CN2021085661W WO2022147922A1 WO 2022147922 A1 WO2022147922 A1 WO 2022147922A1 CN 2021085661 W CN2021085661 W CN 2021085661W WO 2022147922 A1 WO2022147922 A1 WO 2022147922A1
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metal material
gradient
pieces
original
grain sizes
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PCT/CN2021/085661
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English (en)
French (fr)
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陆建勋
程涛
伍博
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深圳技术大学
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Publication of WO2022147922A1 publication Critical patent/WO2022147922A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
    • 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
    • C21D7/00—Modifying the physical properties of iron or steel by deformation
    • C21D7/02—Modifying the physical properties of iron or steel by deformation by cold working
    • 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
    • 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
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • 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
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon

Definitions

  • the present application belongs to the technical field of precision machining, and in particular, relates to a gradient nanostructure metal material and a preparation method thereof.
  • the properties of metal materials determine the scope of application of the material and the rationality of its application.
  • the properties of metal materials are mainly divided into four aspects, namely: mechanical properties, chemical properties, physical properties, and technological properties. Based on the excellent performance of metal materials in four aspects, their application fields are becoming more and more extensive. However, a large number of studies have shown that when the internal grain size of the metal material is reduced and the material strength is enhanced, the material toughness will be greatly reduced, which is a long-standing problem in the field of metal materials research, and the existence of this problem also limits the metal The versatility of the material.
  • One of the strategies to improve the toughness of materials is to change the internal microstructure and introduce one or more gradient-distributed microstructures inside the material to avoid the sudden change of properties due to the variation of feature size such as grain size, and effectively solve the problem of strength and toughness.
  • the "inverted relationship" puzzle, such materials are called gradient nanostructured materials.
  • the artificially prepared gradient nanostructured metals mainly introduce gradient nanostructures into the mature metal materials, thereby improving their strength and toughness.
  • the purpose of this application is to provide a gradient nanostructure material and a preparation method thereof, aiming to solve the problem that the processing method in the prior art can only form a partial gradient nanostructure on the surface of the metal material, resulting in the inability to simultaneously improve the toughness and strength of the metal material The problem.
  • the present application provides a method for preparing a gradient nanostructured metal material, comprising the following steps:
  • n pieces of original metal material and using the equal-diameter angular extrusion process to extrude the original metal materials in different passes to obtain n pieces of metal material with different grain sizes, wherein n is not less than 3;
  • n pieces of the metal material are respectively cut by a wire cutting process, and the impurity removal treatment is carried out to obtain n pieces of metal material sheets with different grain sizes;
  • the original metal material sheet and the coarse-grained metal material sheet are provided, and n pieces of the metal material sheet are stacked and arranged in sequence according to the size of the crystal grains, and the stacking process is sequentially performed by the cumulative stacking welding process to prepare the gradient nanostructure metal material.
  • the present application provides a gradient nanostructured metal material, the gradient nanostructured metal material is a bulk gradient nanostructured metal material, and the gradient nanostructured metal material is composed of different crystals stacked in sequence from the surface to the core.
  • a metal material sheet with grain size, the grain size is different grain sizes from small to large in order from the surface to the core.
  • the first aspect of the present application provides a method for preparing a gradient nanostructured metal material.
  • the original metal material is repeatedly extruded for several times by an equal-diameter angular extrusion process, and then metal materials with different grain sizes are obtained.
  • the size of the obtained crystal grains can be controlled, which can be adjusted according to the needs; and then through the wire cutting process, the metal material sheets with the same size and different grain sizes are obtained, and then the cumulative stacking is used.
  • the welding method is to roll two metal material sheets of the same size in turn, and after the cycle is repeated several times, the sheets can be stacked and welded to obtain a metal material with a gradient nanostructure, which is a short distance from the surface in the prior art.
  • the preparation method is based on equal-diameter angular extrusion and cumulative stack welding.
  • the metal materials obtained by the synergy of the two methods have gradient nanostructures as a whole, which can be controlled according to actual needs.
  • the obtained metal materials have different gradient nanostructures, and the size of the crystal grains can also be controlled. Therefore, the preparation method is simple and easy to operate, and has high flexibility.
  • the gradient nanostructures of metal materials and The grain size is controlled, so that the obtained gradient nano-structured metal material can ensure high material strength and material toughness at the same time, so as to meet the use requirements and expand the use range.
  • a second aspect of the present application provides a gradient nanostructured metal material, wherein the gradient nanostructured metal material is a bulk gradient nanostructured metal material, and the gradient nanostructured metal material is composed of different crystals stacked in sequence from the surface to the core.
  • the metal material sheet with grain size, the grain size from the surface to the core is in order of different grain sizes from small to large; because the gradient nanostructured metal material has a gradient nanostructure as a whole, so that the obtained gradient nanostructured metal material can be simultaneously It is guaranteed to have high material strength and material toughness, and at the same time, the gradient nanostructure and grain size of the gradient nanostructure metal material can be adjusted, and the obtained product has wide applicability and can be set according to actual needs, realizing a wide range of applications.
  • FIG. 1 is a flowchart of a method for preparing a gradient nanostructured metal material provided in an embodiment of the present application.
  • FIG. 2 is a device diagram of an equal-diameter angular extrusion process provided by an embodiment of the present application.
  • FIG. 3 is an operation diagram of the equal-diameter angular extrusion process provided by the embodiment of the present application.
  • FIG. 4 is an operation diagram of the wire cutting process provided by the embodiment of the present application.
  • FIG. 5 is a crystal grain microstructure diagram of the pure copper metal material processed by four equal-diameter angular extrusion processes provided in Example 1 of the present application.
  • FIG. 6 is a crystal grain microstructure diagram of the pure copper metal material processed by the 6-pass equal-diameter angular extrusion process provided in Example 1 of the present application.
  • FIG. 7 is a crystal grain microstructure diagram of the pure copper metal material processed by the 8-pass equal-diameter angular extrusion process provided in Example 1 of the present application.
  • FIG. 8 is a structural diagram of the pure copper gradient nanostructured metal material provided in Example 1 of the present application.
  • FIG. 9 is a grain microstructure diagram of the 6061 aluminum alloy metal material provided in Example 2 of the present application after being processed by four equal-diameter angular extrusion processes.
  • FIG. 10 is a grain microstructure diagram of the 6061 aluminum alloy metal material provided in Example 2 of the present application after 6 passes of equal-diameter angular extrusion processes.
  • FIG. 11 is a grain microstructure diagram of the 6061 aluminum alloy metal material provided in Example 2 of the present application after being processed by 8 passes of equal-diameter angular extrusion.
  • FIG. 12 is a structural diagram of the 6061 aluminum alloy gradient nanostructured metal material provided in Example 2 of the present application.
  • At least one means one or more, and “plurality” means two or more.
  • At least one item(s) below” or similar expressions refer to any combination of these items, including any combination of single item(s) or plural items(s).
  • At least one (one) of a, b, or c or, “at least one (one) of a, b, and c" can mean: a, b, c, a-b (i.e. a and b), a-c, b-c, or a-b-c, where a, b, c can be single or multiple respectively.
  • the weight of the relevant components mentioned in the description of the examples of this application can not only refer to the specific content of each component, but also can represent the proportional relationship between the weights of the components. It is within the scope disclosed in the description of the embodiments of the present application that the content of the ingredients is scaled up or down.
  • the mass described in the description of the embodiments of the present application may be a mass unit known in the chemical field, such as ⁇ g, mg, g, and kg.
  • first and second are only used for descriptive purposes to distinguish objects such as substances from each other, and cannot be understood as indicating or implying relative importance or implying the number of indicated technical features.
  • first XX may also be referred to as the second XX
  • second XX may also be referred to as the first XX .
  • a feature defined as “first” or “second” may expressly or implicitly include one or more of that feature.
  • a first aspect of the embodiments of the present application provides a method for preparing a gradient nanostructured metal material, as shown in FIG. 1 , including the following steps:
  • n pieces of the metal material are respectively cut by a wire cutting process, and the impurity removal treatment is carried out to obtain n pieces of metal material sheets with different grain sizes;
  • the original metal material sheet and the coarse-grained metal material sheet are provided, and n pieces of the metal material sheet are stacked and arranged in sequence according to the size of the crystal grains, and the stacking process is sequentially performed by the cumulative stacking welding process to prepare the gradient nanostructure metal material.
  • the first aspect of the present application provides a method for preparing a gradient nanostructured metal material.
  • the original metal material is repeatedly extruded for several times by an equal-diameter angular extrusion process, and then metal materials with different grain sizes are obtained.
  • the size of the obtained crystal grains can be controlled, which can be adjusted according to the needs; and then through the wire cutting process, the metal material sheets with the same size and different grain sizes are obtained, and then the cumulative stacking is used.
  • the welding method is to roll two metal material sheets of the same size in turn, and after the cycle is repeated several times, the sheets can be stacked and welded to obtain a metal material with a gradient nanostructure, which is a short distance from the surface in the prior art.
  • the preparation method is based on equal-diameter angular extrusion and cumulative stack welding.
  • the metal materials obtained by the synergy of the two methods have gradient nanostructures as a whole, which can be controlled according to actual needs.
  • the obtained metal materials have different gradient nanostructures, and the size of the crystal grains can also be controlled. Therefore, the preparation method is simple and easy to operate, and has high flexibility.
  • the gradient nanostructures of metal materials and The grain size is controlled, so that the obtained gradient nano-structured metal material can ensure high material strength and material toughness at the same time, so as to meet the use requirements and expand the use range.
  • n pieces of original metal materials are provided, and the types of original metal materials are not limited, and any type of original metal materials can be selected for testing as required.
  • the original metal material is selected from pure copper material or aluminum alloy material.
  • the original metal material can be selected from, but not limited to, rod-shaped material and block-shaped material, and the specific shape can be selected according to specific needs without limitation.
  • a rod-shaped original metal material is selected for testing, and the diameter of the rod-shaped original metal material is selected from 15 to 20 mm, the average grain size on the surface is 7 ⁇ 10 ⁇ m.
  • n is not less than 3.
  • n is selected from but not including 3, 4, 5, 6, 7, 8, 9, 10.
  • the original metal material is subjected to different passes of extrusion treatment by using an equal-diameter angular extrusion process to obtain n pieces of metal material with different grain sizes.
  • the equal-diameter angular extrusion process refers to a large plastic deformation processing method that uses pure shear deformation to refine crystal grains.
  • the specific process device is shown in Figure 2.
  • Channels with the same shape and the same cross-sectional area intersect each other at a certain angle.
  • the inner mold corner where the two channels intersect is ⁇
  • the mold center angle where the channels intersect is ⁇
  • the inner mold corner where the channels intersect is ⁇ , 90° ⁇ 120°
  • the central angle of the mold where the channels intersect is equal to ⁇ , and 60° ⁇ 90°.
  • the choice of the angle can directly control the intensity of the deformation process of the material, and then control the degree of refinement of the material. Different processing angles will affect the grain size of the obtained material.
  • the inner mold corner ⁇ where the channels intersect is 90°; the central angle ⁇ of the mold where the channels intersect is 90° to perform equal-diameter angular extrusion processing, and processing at this angle can obtain a large-angle grain boundary crystal structure , ensuring the formation of nanostructures.
  • the step of extruding the original metal material in different passes by using the equal-diameter angular extrusion process includes the following steps: putting the original original metal material into the vertical channel of the mold, and under the pressure of the indenter. Under the action, the original metal material is extruded from the vertical channel to the horizontal channel to complete the extrusion process. As shown in Figure 3, when passing through the intersection (bend) of the two channels, the original metal material produces approximately ideal pure shear deformation in the main deformation zone. Through the equal-diameter angular extrusion process, it can ensure that the original metal material does not change the cross-sectional shape and size.
  • the cumulative superposition of the strains of each pass of deformation can obtain a larger total strain.
  • the internal larger grains of the original metal material are broken and refined into sub-micron or even nano-scale ultra-fine grains, and large deformations occur to form microstructures with different grain fineness.
  • the original metal material in the step of extruding the original metal material in different passes by using an equal-diameter angular extrusion process, after each extrusion, the original metal material does not rotate, and the next pass of extrusion is directly performed.
  • the treatment can ensure that the obtained original metal material achieves the accumulation and superposition of strain at the same position, forming a larger total strain amount.
  • the extruding temperature is 20-25° C., and the extruding process is performed at room temperature. , to ensure a good degree of grain refinement during the deformation process of the original metal material. If the extrusion temperature is too high, the internal energy inside the metal material will be higher, and the thermal motion of the atoms will be more intense. The degree of crystallization is reduced, and the purpose of fine crystallization cannot be achieved.
  • different passes are respectively carried out, wherein 1 to 8 arbitrary passes of extrusion are carried out respectively.
  • Pressing treatment; controlling the number of passes of the extrusion treatment can further control the size of the grain size of the obtained metal material. If the number of passes of the extrusion treatment is more, the grain size will be continuously refined and homogenized. Among them, when the extrusion pass reaches the 8th pass, the grain size reaches the minimum, even if the extrusion pass is increased again, the grain size does not change much.
  • the average grain size of the materials obtained by extruding the same pass will also be different.
  • the number of processing passes can be further determined according to the needs.
  • the metal material is extruded for 4 passes, 6 passes, and 8 passes, respectively.
  • the original metal material is selected from pure copper materials, and 3 pieces of pure copper materials are provided, and the 3 pieces of pure copper materials are respectively subjected to 4 passes and 6 passes through an equal-diameter angular extrusion process.
  • 8 passes of extrusion treatment wherein the extrusion treatment temperature is room temperature 25°C, the inner die corner ⁇ where the channels intersect is 90°; the die center angle ⁇ where the channels intersect is 90° for equal-diameter angle extrusion treatment .
  • the average grain size of the pure copper material subjected to 4 passes of extrusion treatment is 0.95 ⁇ m
  • the average grain size of pure copper material extruded in 6 passes is 0.79 ⁇ m
  • the average grain size of pure copper material extruded in 8 passes is 0.51 ⁇ m.
  • the original metal material is selected from 6061 aluminum alloy materials, three pieces of 6061 aluminum alloy materials are provided, and the three pieces of 6061 aluminum alloy materials are respectively subjected to four passes, 6 passes and 8 passes of extrusion treatment, wherein the extrusion treatment temperature is room temperature 25°C, the inner mold corner ⁇ where the channels intersect is 90°; the mold center angle ⁇ where the channels intersect is 90° for equal diameter Angular extrusion treatment.
  • the average grain size of the 6061 aluminum alloy material subjected to 4 passes of extrusion treatment is 0.8 ⁇ m
  • the average grain size of 6061 aluminum alloy material extruded in 6 passes is 0.7 ⁇ m
  • the average grain size of 6061 aluminum alloy material processed by 8 passes is 0.45 ⁇ m.
  • step S02 the n pieces of metal material are respectively cut by wire cutting process, and the impurity removal process is carried out to obtain n pieces of metal material sheets with different grain sizes, and the wire cutting process is carried out for the subsequent cumulative lap welding process.
  • the impurity removal process is carried out to obtain n pieces of metal material sheets with different grain sizes
  • the wire cutting process is carried out for the subsequent cumulative lap welding process.
  • the step of separately cutting n pieces of metal materials by using a wire cutting process includes: vertically fixing n pieces of metal materials with different grain sizes on the equipment, and using the wire cutting process.
  • Cutting process from metal material includes: the voltage is 70 ⁇ 75 V, the current is 0.4 ⁇ 0.5 A, the pulse width ratio is (3 ⁇ 3.5):4.
  • the wire cutting process in the step of separately cutting the n pieces of metal material by a wire cutting process, includes: a voltage of 70 V, the current is 0.4 A, the pulse width ratio is 3:4.
  • the impurity removal treatment is performed after the cutting treatment, and the impurity removal treatment is mainly to remove the oxide layer and surface dirt on the surface of the cut material, so as to make the sheet clean and tidy.
  • the impurity removal treatment includes sanding treatment with sandpaper and ultrasonic cleaning treatment with organic solvent. Among them, 1500 ⁇ 2000 mesh sandpaper is selected for grinding treatment. The grinding treatment is to rub all the end faces of the obtained sheet until the surface oxide layer is bright; the grinding treatment time is 15 ⁇ 20 minutes to ensure that all the end faces of the sheet are rubbed to the surface. The oxide layer is bright.
  • ultrasonic cleaning with an organic solvent can remove the oxide layer and dirt.
  • the ultrasonic cleaning treatment time is 10 to 15 minutes.
  • the thin plate is ultrasonically cleaned to completely clean the oxide layer and dirt on the surface.
  • the organic solvent is selected from but not limited to absolute ethanol and acetone.
  • the length of the sheet is 50-100 mm, width is 10 ⁇ 20 mm, the thickness is 0.5 ⁇ 1 mm. Controlling the size of the sheet is beneficial to the subsequent cumulative lap welding process.
  • step S03 the original metal material sheet and the coarse-grained metal material sheet are provided, and the n metal material sheets are stacked in sequence according to the size of the crystal grains, and the stacking process is sequentially performed by the cumulative stacking welding process to prepare the gradient nanostructure.
  • the cumulative stacking welding process can stack two sheets of equal size at a certain temperature and automatically weld them together, and then repeat the same process for repeated stacking, rolling and welding, so as to refine the structure of the material.
  • the inclusions are evenly distributed, which breaks through the limitation of the traditional rolling reduction, and can continuously prepare ultra-fine-grained metal materials such as thin plates, so that the thickness of the obtained materials is thinner, and at the same time, large pieces of ultra-fine-grained metal materials can be produced.
  • the original metal material sheet and the coarse-grained metal material sheet are the original metal material provided by the equal-diameter angle extrusion process, and the original metal material is subjected to wire cutting pretreatment to obtain the same as the metal material.
  • the metal material sheet with the same sheet specification; the coarse-grained metal material sheet refers to the coarse-grained metal material with larger grain size obtained by coarse-graining the original metal material.
  • the average grain size of the coarse-grained metal material is not specified. Limited requirements, as long as the degree of coarse crystals can be reached.
  • the original metal material sheet and the coarse-grained metal material sheet are provided, and the n metal material sheets are stacked in sequence according to the size of the crystal grains, and the stacking process is sequentially performed by the cumulative stacking welding process to prepare the gradient nanostructured metal material.
  • the thin plates are stacked and arranged in sequence according to the grain size from small to large, and the stacking process is performed in sequence by the cumulative stacking welding process.
  • the number of passes of the cumulative lap welding process is further determined, wherein the passes of the lap welding are selected from, but not limited to, 3 times, 4 times, and 5 times.
  • the passes of the lap welding are selected from, but not limited to, 3 times, 4 times, and 5 times.
  • the cumulative stacking rolling process is used to sequentially perform stacking processing.
  • the method includes: rolling the first metal material sheet and the second metal material sheet to form a first composite metal material; subjecting the first composite metal material and the third metal material sheet to rolling processing to form a second composite metal material; The second composite metal material and the fourth metal material sheet are rolled to form a third composite metal material; the third composite metal material and the fifth metal material sheet are rolled to form a gradient nanostructure metal material.
  • the step of sequentially performing the stacking process using the cumulative stacking welding process includes: providing a two-high rolling mill with a maximum rolling force of 200-250 t, rolling speed 0.5 ⁇ 1.0
  • the lamination process is carried out under the condition of m/s, in which the diameter of the rolls of the two-roll mill is 230 ⁇ 250 mm, the length of the roller is 200 ⁇ 250 mm. Controlling the maximum rolling force and rolling speed of the stacking process can ensure that the obtained metal material has a gradient nanostructure as a whole, so that the obtained gradient nanostructure metal material can simultaneously ensure high material strength and material toughness, so as to achieve Use demand, expand the scope of use.
  • the step of sequentially performing the stacking process by adopting the cumulative stacking welding process includes: providing a two-high rolling mill with a maximum rolling force of 200 t, rolling speed 0.5
  • the lamination process is carried out under the condition of m/s, in which the diameter of the rolls of the two-roll mill is 230 mm with a roll length of 20 mm.
  • a second aspect of the embodiments of the present application provides a gradient nanostructured metal material, the gradient nanostructured metal material is a bulk gradient nanostructured metal material, and the gradient nanostructured metal material is sequentially stacked from the surface to the core of different grain sizes.
  • the metal material sheet, the grain size from the surface to the core is different grain size from small to large.
  • a second aspect of the present application provides a gradient nanostructured metal material, wherein the gradient nanostructured metal material is a bulk gradient nanostructured metal material, and the gradient nanostructured metal material is sequentially stacked from the surface to the core of metals with different grain sizes
  • the material thin plate, the grain size from the surface to the core is in order of different grain sizes from small to large; because the gradient nanostructured metal material has a gradient nanostructure as a whole, the gradient nanostructured metal material can be obtained at the same time.
  • the gradient nanostructure and grain size of the gradient nanostructured metal material can be adjusted, and the obtained product has wide applicability and can be set according to actual needs, thus realizing a wide range of applications.
  • the thickness of the gradient nanostructured metal material is 0.5-1 mm
  • the obtained gradient nanostructured metal material also has a plurality of gradient nanostructured grains in a thinner structure, so that the obtained gradient nanostructured metal material can ensure high material strength and material toughness at the same time.
  • the preparation method of pure copper gradient nanostructure metal material comprises the following steps:
  • the virgin material is selected from the diameter of 15 mm, the average grain size is about 7 ⁇ m pure copper bar;
  • the three pure copper bars were extruded for 4 passes, 6 passes and 8 passes respectively by the equal-diameter angular extrusion process to obtain 3 metal materials with different grain sizes;
  • the treatment temperature is room temperature 25°C, the inner mold corner ⁇ where the channels intersect is 90°; the mold central angle ⁇ where the channels intersect is 90° for equal-diameter angular extrusion treatment.
  • the average grain size of the pure copper material subjected to 4 passes of extrusion treatment is 0.95 ⁇ m
  • the average grain size of pure copper material extruded in 6 passes is 0.79 ⁇ m
  • the average grain size of pure copper material extruded in 8 passes is 0.51 ⁇ m;
  • 3 pieces of metal materials with different grain sizes are cut separately by wire cutting process, wherein the wire cutting process includes: the voltage is 70 V, the current is 0.4 A, the pulse width ratio is 3:4; then carry out the impurity removal treatment.
  • the impurity removal treatment is to use 1500 mesh sandpaper for grinding treatment for 15 minutes, and use absolute ethanol for ultrasonic cleaning treatment for 15 minutes to obtain 3 pieces of metal with different grain sizes.
  • Material sheet, wherein the thickness of the metal material sheet is 50 long mm, width 10mm, thickness 1mm;
  • the coarse-grained pure copper material of ⁇ m is processed by wire cutting to obtain a thickness of 50 mm. mm, width 10mm, thickness is 1mm coarse-grained metal material sheet;
  • the metal material sheets of ⁇ m are stacked in sequence, and the first stacking process is performed to form a first composite metal material; the first composite metal material and the average grain size are 0.95
  • the metal material sheets of ⁇ m are stacked in sequence, and the second stack rolling process is performed to form the second composite metal material; the second composite metal material and the metal material sheets are stacked and arranged in sequence, and the third stack rolling process is performed to form the first composite metal material.
  • the step of stacking includes: providing two rolling mill, at a maximum rolling force of 200 t, rolling speed 0.5
  • the lamination process is carried out under the condition of m/s, in which the diameter of the rolls of the two-roll mill is 230 mm with a roll length of 200 mm.
  • the gradient nanostructured metal material is a bulk gradient nanostructured metal material, and the gradient nanostructured metal material is sequentially stacked from the surface to the core of metal material sheets with different grain sizes, and the grain size is from the surface to the core. 0.51 microns, 0.79 microns, 0.95 microns, 7 microns, 15 microns.
  • the preparation method of 6061 aluminum alloy gradient nanostructure metal material comprises the following steps:
  • the original material is selected from the diameter of 15 mm, the average grain size is about 7 ⁇ m pure copper bar;
  • the three 6061 aluminum alloy bars were extruded for 4 passes, 6 passes and 8 passes respectively by the equal-diameter angular extrusion process to obtain 3 pieces of metal materials with different grain sizes;
  • the temperature of the pressure treatment is room temperature 25°C, the inner die corner ⁇ where the channels intersect is 90°; the central angle ⁇ of the die where the channels intersect is 90° for equal-diameter angular extrusion treatment.
  • the average grain size of the 6061 aluminum alloy material subjected to 4 passes of extrusion treatment is 0.8 ⁇ m
  • the average grain size of 6061 aluminum alloy material extruded in 6 passes is 0.7 ⁇ m
  • the average grain size of 6061 aluminum alloy material processed by 8 passes is 0.45 ⁇ m;
  • Three pieces of metal materials with different grain sizes are cut separately by wire cutting process, wherein the wire cutting process includes: the voltage is 70 V, the current is 0.4 A, the pulse width ratio is 3:4; then carry out the impurity removal treatment.
  • the impurity removal treatment is to use 1500 mesh sandpaper for grinding treatment for 15 minutes, and use absolute ethanol for ultrasonic cleaning treatment for 15 minutes to obtain 3 pieces of metal with different grain sizes.
  • Material sheet, wherein the thickness of the metal material sheet is 50 long mm, width 10mm, thickness 1mm;
  • the step of stacking includes: providing two rolling mill, at a maximum rolling force of 200 t, rolling speed 0.5
  • the lamination process is carried out under the condition of m/s, in which the diameter of the rolls of the two-roll mill is 230 mm with a roll length of 200 mm.
  • the gradient nanostructured metal material is a bulk gradient nanostructured metal material, and the gradient nanostructured metal material is sequentially stacked from the surface to the core of metal material sheets with different grain sizes, and the grain size is from the surface to the core. 0.45 microns, 0.7 microns, 0.8 microns, 7 microns, 20 microns.
  • the microstructure of the pure copper metal material obtained by the equal-diameter angular extrusion process of 4 passes, 6 passes, and 8 passes in Example 1 was characterized by EBSD.
  • the pure copper metal material obtained by the radial angle extrusion process is shown in Figure 5, and the average grain size is 0.95 microns; As shown in Figure 7, the average grain size is 0.79 microns; the pure copper metal material obtained by 8 passes of equal-diameter angular extrusion process is shown in Figure 7, and the average grain size is 0.51 microns.
  • Example 1 Pure copper gradient nanostructured metal material
  • the gradient nanostructured metal material is a metal material sheet with different grain sizes stacked in sequence from the surface to the core, and the grain size is from the surface to the core.
  • the parts are 0.51 microns, 0.79 microns, 0.95 microns, 7 microns, and 15 microns in sequence.
  • the microstructure of the 6061 aluminum alloy metal material obtained by 4 passes, 6 passes, and 8 passes of the equal-diameter angular extrusion process in Example 2 was subjected to EBSD characterization, wherein 4 passes were carried out.
  • the 6061 aluminum alloy metal material obtained by the equal-diameter angular extrusion process is shown in Figure 9, and the average grain size is 0.8 microns; As shown in Figure 10, the average grain size is 0.7 microns; the 6061 aluminum alloy metal material obtained by 8 passes of equal-diameter angular extrusion process is shown in Figure 11, and the average grain size is 0.45 microns.
  • Example 2 6061 aluminum alloy gradient nanostructure metal material is shown in Figure 12.
  • the gradient nanostructure metal material is a metal material sheet with different grain sizes stacked in sequence from the surface to the core, and the grain size is sequentially from the surface to the core. 0.45 microns, 0.7 microns, 0.8 microns, 7 microns, 20 microns.
  • Example 1 The hardness and elongation of the gradient nanostructured metal material prepared in Example 1 and Example 2 were tested respectively, wherein the microhardness of the upper surface layer of the pure copper gradient nanostructured metal material obtained in Example 1 was about HV130, and the most The microhardness of the lower layer is about HV70; the tensile test shows that the elongation of the prepared pure copper gradient nanostructured metal material is significantly higher than that of the ultrafine-grained material and close to the elongation of the coarse-grained material; the 6061 aluminum alloy gradient obtained in Example 2 The microhardness of the upper surface layer of the nanostructured metal material is about HV100, while the microhardness of the bottom layer is about HV60; the tensile test shows that the elongation of the prepared pure copper gradient nanostructured metal material is significantly higher than that of the ultrafine-grained material, which is close to coarse. elongation of the crystalline material.
  • the preparation method of the gradient nano-structured metal material is provided.
  • the preparation method firstly adopts the equal-diameter angular extrusion process to repeatedly extrude the metal material for several passes, and then obtains the metal material with different grain sizes. With different passes, the size of the obtained crystal grains can be controlled and adjusted according to needs; after wire cutting processing, metal material sheets with different grain sizes of the same size are obtained, and then the cumulative stack welding method is used to sequentially Two metal material sheets of the same size are rolled, and after several cycles are repeated, the sheets can be rolled and welded together to obtain a metal material with a gradient nanostructure, which is different from the existing technology with a gradient nanostructure at a small distance from the surface.
  • the preparation method is based on equal-diameter angular extrusion and cumulative stack rolling.
  • the metal materials obtained by the synergy of the two methods have a gradient nanostructure as a whole, and the obtained metal materials can be controlled according to actual needs. Different gradient nanostructures can also control the grain size. Therefore, the preparation method is simple and easy to operate and has great flexibility. According to actual needs, the gradient nanostructure and grain size of metal materials can be further processed. Through the control, the obtained gradient nano-structured metal material can ensure high material strength and material toughness at the same time, so as to meet the use requirements and expand the use range.

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Abstract

一种梯度纳米结构金属材料的制备方法，包括如下步骤：提供n块原始金属材料，采用等径角挤压工艺将原始金属材料分别进行不同道次的挤压处理，得到n块具有不同晶粒尺寸的金属材料，将n块金属材料采用线切割工艺分别进行切割处理，并进行除杂处理，得到n块具有不同晶粒尺寸的金属材料薄板，提供原始金属材料薄板、粗晶金属材料薄板，与n块金属材料薄板按照晶粒尺寸的大小依次层叠设置，采用累积叠轧焊工艺依次进行叠轧处理，得到梯度纳米结构金属材料。一种梯度纳米结构金属材料，从表面至芯部为依次层叠设置的不同晶粒尺寸的金属材料薄板。梯度纳米结构金属材料的制备方法简单方便，灵活性大，得到的梯度纳米结构金属材料具有较高的材料强度和韧性。

Description

梯度纳米结构金属材料及其制备方法 技术领域
本申请属于精密加工技术领域，尤其涉及一种梯度纳米结构金属材料及其制备方法。
 背景技术
金属材料的性能决定着材料的适用范围及应用的合理性。金属材料的性能主要分为四个方面，即：机械性能、化学性能、物理性能、工艺性能。基于金属材料具有较优异的四个方面的性能，其应用领域越来越广泛。然而，大量研究表明，当金属材料内部晶粒尺寸减小、材料强度得到增强时，材料韧性将大大降低，这是金属材料研究领域长期存在的难题，而这一问题的存在，也限制了金属材料的应用广泛性。
通常提高材料韧性的策略之一是改变内部组织微结构，在材料内部引入一种或多种梯度分布的微结构，避免由于特征尺寸如晶粒尺寸变异导致的性能突变，有效解决强度和韧性的“倒置关系”难题，这种材料被称为梯度纳米结构材料。人工制备的梯度纳米结构金属主要在已经发展成熟的金属材料内部引入梯度纳米结构，从而提高其强韧性能力。
现有技术中，一般都是通过表面研磨处理（SMAT）在孪晶诱发塑性（TWIP）钢表面引入大量的塑性变形，使其表面晶粒细化，随着深度的增加，晶粒细化的程度逐渐降低，同时塑性变形也会导致位错演化和孪晶的产生。由于这类工艺是通过对金属材料的表面进行大量的塑性变形，制备的梯度纳米结构材料只局限在距离钢表面约0.1 mm的厚度，得到的金属材料为形成部分梯度纳米结构的材料，无法获得具有块状梯度纳米结构金属材料，因此也限制了金属材料的广泛应用。
 技术问题
本申请的目的在于提供一种梯度纳米结构材料及其制备方法，旨在解决现有技术中的加工方法仅能使金属材料的表面形成部分梯度纳米结构，导致无法同时提高金属材料的韧性和强度的问题。
 技术解决方案
为实现上述申请目的，本申请采用的技术方案如下：
第一方面，本申请提供一种梯度纳米结构金属材料的制备方法，包括如下步骤：
提供n块原始金属材料，采用等径角挤压工艺将所述原始金属材料分别进行不同道次的挤压处理，得到n块具有不同晶粒尺寸的金属材料，其中，n不少于3；
将n块所述金属材料采用线切割工艺分别进行切割处理，并进行除杂处理，得到n块具有不同晶粒尺寸的金属材料薄板；
提供原始金属材料薄板、粗晶金属材料薄板，与n块所述金属材料薄板按照晶粒尺寸的大小依次层叠设置，采用累积叠轧焊工艺依次进行叠轧处理，制备得到梯度纳米结构金属材料。
第二方面，本申请提供一种梯度纳米结构金属材料，所述梯度纳米结构金属材料为块状梯度纳米结构金属材料，所述梯度纳米结构金属材料从表面至芯部为依次层叠设置的不同晶粒尺寸的金属材料薄板，所述晶粒尺寸从表面至芯部依次为从小到大的不同晶粒尺寸。
 有益效果
本申请第一方面提供的梯度纳米结构金属材料的制备方法，该制备方法先采用等径角挤压工艺将原始金属材料进行反复挤压若干道次后获得具有不同晶粒尺寸的金属材料，通过控制进行不同道次的挤压处理，可以控制得到的晶粒尺寸的大小，可根据需要进行调整；再经过线切割处理，得到大小一致的不同晶粒尺寸的金属材料薄片，再利用累积叠轧焊的方法依次将两块大小一致的金属材料薄片进行轧制，循环反复几次后就可以把薄片叠轧焊和，得到具有梯度纳米结构的金属材料，与现有技术中距离表面一小段距离具有梯度纳米结构的金属材料相比，该制备方法是基于等径角挤压和累积叠轧焊工艺，采用两种方法协同作用得到的金属材料整体均具有梯度纳米结构，可根据实际需要，控制得到的金属材料具有不同的梯度纳米结构，同时也可对晶粒尺寸的大小进行控制，因此，该制备方法简便易操作，灵活性大，可根据实际需求，进一步对金属材料的梯度纳米结构以及晶粒尺寸大小进行控制，使得到的梯度纳米结构金属材料能够同时保证具有较高的材料强度以及材料韧性，以实现使用需求，扩大了使用范围。
本申请第二方面提供的一种梯度纳米结构金属材料，所述梯度纳米结构金属材料为块状梯度纳米结构金属材料，所述梯度纳米结构金属材料从表面至芯部为依次层叠设置的不同晶粒尺寸的金属材料薄板，所述晶粒尺寸从表面至芯部依次为从小到大的不同晶粒尺寸；由于梯度纳米结构金属材料整体具有梯度纳米结构，使得到的梯度纳米结构金属材料能够同时保证具有较高的材料强度以及材料韧性，同时该梯度纳米结构金属材料的梯度纳米结构以及晶粒尺寸均可调节，得到的产品适用性广，可根据实际的需求进行设置，实现了广泛应用。
 附图说明
为了更清楚地说明本申请实施例中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本申请的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1是本申请实施例提供的梯度纳米结构金属材料的制备方法的流程图。
图2是本申请实施例提供的等径角挤压工艺的装置图。
图3是本申请实施例提供的等径角挤压工艺的操作图。
图4是本申请实施例提供的线切割工艺的操作图。
图5是本申请实施例1提供的经过4个道次等径角挤压工艺处理后的纯铜金属材料的晶粒微结构图。
图6是本申请实施例1提供的经过6个道次等径角挤压工艺处理后的纯铜金属材料的晶粒微结构图。
图7是本申请实施例1提供的经过8个道次等径角挤压工艺处理后的纯铜金属材料的晶粒微结构图。
图8是本申请实施例1提供的纯铜梯度纳米结构金属材料的结构图。
图9是本申请实施例2提供的经过4个道次等径角挤压工艺处理后的6061铝合金金属材料的晶粒微结构图。
图10是本申请实施例2提供的经过6个道次等径角挤压工艺处理后的6061铝合金金属材料的晶粒微结构图。
图11是本申请实施例2提供的经过8个道次等径角挤压工艺处理后的6061铝合金金属材料的晶粒微结构图。
图12是本申请实施例2提供的6061铝合金梯度纳米结构金属材料的结构图。
 本发明的实施方式
为了使本申请要解决的技术问题、技术方案及有益效果更加清楚明白，以下结合实施例，对本申请进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本申请，并不用于限定本申请。
本申请中，术语“和/或”，描述关联对象的关联关系，表示可以存在三种关系，例如，A和/或B，可以表示：单独存在A，同时存在A和B，单独存在B的情况。其中A，B可以是单数或者复数。字符“/”一般表示前后关联对象是一种“或”的关系。
本申请中，“至少一个”是指一个或者多个，“多个”是指两个或两个以上。“以下至少一项(个)”或其类似表达，是指的这些项中的任意组合，包括单项（个）或复数项（个）的任意组合。例如，“ a,b,或c中的至少一项（个）”，或，“a,b,和c中的至少一项（个）”，均可以表示：a, b, c, a-b（即a和b）, a-c, b-c, 或a-b-c，其中a,b,c分别可以是单个，也可以是多个。
应理解，在本申请的各种实施例中，上述各过程的序号的大小并不意味着执行顺序的先后，部分或全部步骤可以并行执行或先后执行，各过程的执行顺序应以其功能和内在逻辑确定，而不应对本申请实施例的实施过程构成任何限定。
在本申请实施例中使用的术语是仅仅出于描述特定实施例的目的，而非旨在限制本申请。在本申请实施例和所附权利要求书中所使用的单数形式的“一种”、“所述”和“该”也旨在包括多数形式，除非上下文清楚地表示其他含义。
本申请实施例说明书中所提到的相关成分的重量不仅仅可以指代各组分的具体含量，也可以表示各组分间重量的比例关系，因此，只要是按照本申请实施例说明书相关组分的含量按比例放大或缩小均在本申请实施例说明书公开的范围之内。具体地，本申请实施例说明书中所述的质量可以是µg、mg、g、kg等化工领域公知的质量单位。
术语“第一“、“第二”仅用于描述目的，用来将目的如物质彼此区分开，而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。例如，在不脱离本申请实施例范围的情况下，第一XX也可以被称为第二XX，类似地，第二XX也可以被称为第一XX 。由此，限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征。
本申请实施例第一方面提供一种梯度纳米结构金属材料的制备方法，如图1所示，包括如下步骤：
S01. 提供n块原始金属材料，采用等径角挤压工艺将所述原始金属材料分别进行不同道次的挤压处理，得到n块具有不同晶粒尺寸的金属材料，其中，n不少于3；
S02. 将n块所述金属材料采用线切割工艺分别进行切割处理，并进行除杂处理，得到n块具有不同晶粒尺寸的金属材料薄板；
S03. 提供原始金属材料薄板、粗晶金属材料薄板，与n块所述金属材料薄板按照晶粒尺寸的大小依次层叠设置，采用累积叠轧焊工艺依次进行叠轧处理，制备得到梯度纳米结构金属材料。
本申请第一方面提供的梯度纳米结构金属材料的制备方法，该制备方法先采用等径角挤压工艺将原始金属材料进行反复挤压若干道次后获得具有不同晶粒尺寸的金属材料，通过控制进行不同道次的挤压处理，可以控制得到的晶粒尺寸的大小，可根据需要进行调整；再经过线切割处理，得到大小一致的不同晶粒尺寸的金属材料薄片，再利用累积叠轧焊的方法依次将两块大小一致的金属材料薄片进行轧制，循环反复几次后就可以把薄片叠轧焊和，得到具有梯度纳米结构的金属材料，与现有技术中距离表面一小段距离具有梯度纳米结构的金属材料相比，该制备方法是基于等径角挤压和累积叠轧焊工艺，采用两种方法协同作用得到的金属材料整体均具有梯度纳米结构，可根据实际需要，控制得到的金属材料具有不同的梯度纳米结构，同时也可对晶粒尺寸的大小进行控制，因此，该制备方法简便易操作，灵活性大，可根据实际需求，进一步对金属材料的梯度纳米结构以及晶粒尺寸大小进行控制，使得到的梯度纳米结构金属材料能够同时保证具有较高的材料强度以及材料韧性，以实现使用需求，扩大了使用范围。
在步骤S01中，提供n块原始金属材料，原始金属材料的种类没有限制，可以根据需要选择任意种类的原始金属材料进行试验。在本发明具体实施例中，原始金属材料选自纯铜材料或铝合金材料。
其中，原始金属材料可选自但不限于棒状材料、块状材料，具体的形状可根据具体的需求进行选择，没有限制。在一些实施例中，选择棒状原始金属材料进行试验，棒状原始金属材料的直径选自15~20 mm，表面平均晶粒大小为7~10 μm。
进一步的，n不少于3，为了保证得到的金属材料具有梯度纳米结构，因此，至少提供3块金属材料分别进行不同道次的挤压处理，得到3块具有不同晶粒尺寸的金属材料，在后续材料制备过程中方能呈现梯度纳米结构。在一些实施例中，n选自但不包括3、4、5、6、7、8、9、10。
进一步的，采用等径角挤压工艺将原始金属材料分别进行不同道次的挤压处理，得到n块具有不同晶粒尺寸的金属材料。
其中，等径角挤压工艺是指利用纯剪切变形细化晶粒的大塑性变形加工方法，具体的工艺处理的装置如图2所示，等径角挤压工艺的模具是由两个具有相同形状且横截面积相等的通道按照一定的角度相互交截组成的，两通道相交的内模具拐角为Φ，通道相交的模具圆心角为Ψ，通道相交的内模具拐角为Φ，90°≤Φ≤120°；通道相交的模具圆心角等于Ψ，且60°≤Ψ≤90°。角度的选择能够直接控制材料变形过程中的强烈程度，进而控制材料的细化程度，不同的处理角度会影响得到的材料的晶粒大小的情况。
在一些实施例中，通道相交的内模具拐角Φ为90°；通道相交的模具圆心角Ψ为90°进行等径角挤压处理，采用该角度进行处理能够得到大角度的晶界的晶结构，保证形成纳米结构。
进一步的，采用等径角挤压工艺将原始金属材料分别进行不同道次的挤压处理的步骤中，包括如下步骤：将原始原始金属材料放入模具的垂直通道中，在压头的压力的作用下，原始金属材料从垂直通道被挤压到水平通道，完成挤压处理。如图3所示，当经过两通道的相交处（弯曲部位）时，原始金属材料在主要变形区产生近似理想的纯剪切变形。通过等径角挤压工艺的处理，能够保证原始金属材料在横截面形状和尺寸大小不改变的情况下，由于挤压变形处理，每道次变形的应变量累积叠加可得到较大的总应变量，使原始金属材料的内部较大的晶粒破碎细化成亚微米甚至纳米级的超细晶晶粒，发生较大的变形，形成不同晶粒细度的组织结构。
在一些实施例中，采用等径角挤压工艺将原始金属材料分别进行不同道次的挤压处理的步骤中，每次挤压后，原始金属材料不旋转，直接进行下一道次的挤压处理，能够保证得到的原始金属材料在相同位置达到应变累积叠加，形成较大的总应变量。
在一些实施例中，采用等径角挤压工艺将原始金属材料分别进行不同道次的挤压处理的步骤中，挤压处理的温度为20~25℃，采用在室温条件下进行挤压处理，保证原始金属材料的变形过程中晶粒的细化程度较好。若挤压处理的温度过高，则金属材料内部的内能越高，原子的热运动越剧烈，但过高的温度会导致晶粒变形过快，不利于大角度晶界的形成，导致细晶化程度降低，无法实现细晶化的目的。
在一些实施例中，采用等径角挤压工艺将原始金属材料分别进行不同道次的挤压处理的步骤中，分别进行不同道次的处理，其中，分别进行1~8任意道次的挤压处理；控制挤压处理的道次，能够进一步控制得到的金属材料的晶粒尺寸的大小，若挤压处理的道次越多，晶粒尺寸不断细化和均匀化。其中，当挤压至第8个道次时，晶粒尺寸达到最小，即使挤压道次再增加，晶粒尺寸变化不大。在挤压处理的过程中，由于提供的金属材料的种类不同，挤压相同的道次得到的材料的平均晶粒尺寸也会存在差异。
在具体使用过程中可根据需求进一步确定处理的道次。在本发明具体实施例中，金属材料分别进行4个道次、6个道次、8个道次的挤压处理。
在本发明一具体实施例中，原始金属材料选自纯铜材料，提供了3块纯铜材料，采用等径角挤压工艺将3块纯铜材料分别进行4个道次、6个道次、8个道次的挤压处理，其中，挤压处理的温度为室温25℃，通道相交的内模具拐角Φ为90°；通道相交的模具圆心角Ψ为90°进行等径角挤压处理。进一步的，进行4个道次挤压处理的纯铜材料的平均晶粒尺寸为0.95 μm，6个道次挤压处理的纯铜材料的平均晶粒尺寸为0.79 μm，8个道次挤压处理的纯铜材料的平均晶粒尺寸为0.51 μm。
在本发明另一具体实施例中，原始金属材料选自6061铝合金材料，提供了3块6061铝合金材料，采用等径角挤压工艺将3块6061铝合金材料分别进行4个道次、6个道次、8个道次的挤压处理，其中，挤压处理的温度为室温25℃，通道相交的内模具拐角Φ为90°；通道相交的模具圆心角Ψ为90°进行等径角挤压处理。进一步的，进行4个道次挤压处理的6061铝合金材料的平均晶粒尺寸为0.8 μm，6个道次挤压处理的6061铝合金材料的平均晶粒尺寸为0.7 μm，8个道次挤压处理的6061铝合金材料的平均晶粒尺寸为0.45 μm。
在步骤S02中，将n块金属材料采用线切割工艺分别进行切割处理，并进行除杂处理，得到n块具有不同晶粒尺寸的金属材料薄板，进行线切割工艺为后续累积叠轧焊处理做准备工作，通过将得到的不同晶粒尺寸的金属材料切割形成相同厚度，相同大小的薄片，才有利于后续进行累积叠轧焊处理，进而重新组织形成具有纳米梯度结构的材料。
进一步的，将n块金属材料采用线切割工艺分别进行切割处理的步骤中，如附图4所示，包括：将n块不同晶粒尺寸的金属材料分别垂直固定在设备上，利用线切割工艺从金属材料进行切割处理。进一步的，线切割工艺包括：电压为70~75 V，电流为0.4~0.5 A，脉宽比为（3~3.5）：4。通过控制线切割工艺的条件，能够进一步保证切割得到的金属材料薄板尺寸统一，且表面的粗糙度保护较好，有利于进行后续累积叠轧焊处理。
在一些实施例中，将n块金属材料采用线切割工艺分别进行切割处理的步骤中，线切割工艺包括：电压为70 V，电流为0.4 A，脉宽比为3：4。
进一步的，在切割处理之后进行除杂处理，除杂处理主要是除去切割得到的材料表面的氧化层和表面脏污，使薄板干净整洁。
在一些实施例中，除杂处理包括采用砂纸进行打磨处理，采用有机溶剂进行超声清洗处理。其中，选择1500~2000目的砂纸进行打磨处理，打磨处理为将得到的薄板的所有端面进行摩擦至表面氧化层光亮；打磨处理的时间为15~20分钟，保证将薄板的所有端面进行摩擦至表面氧化层光亮。
进一步，采用有机溶剂进行超声清洗，能够去除氧化层及脏污，超声清洗处理的时间为10~15分钟，将薄板进行超声清洗处理，使表面的氧化层及脏污完全清洗噶经。其中，有机溶剂选自但不限于无水乙醇、丙酮。
在一些实施例中，薄板的长度为50~100 mm，宽度为10~20 mm，厚度为0.5~1 mm。控制薄板的尺寸大小，有利于后续的累积叠轧焊处理。
在步骤S03中，提供原始金属材料薄板、粗晶金属材料薄板，与n块金属材料薄板按照晶粒尺寸的大小依次层叠设置，采用累积叠轧焊工艺依次进行叠轧处理，制备得到梯度纳米结构金属材料。累积叠轧焊工艺能将尺寸相等的两块薄板材料在一定温度下叠轧并使其自动焊合，然后重复进行相同的工艺反复叠片、轧制焊接，从而使材料的组织得到细化，夹杂物均匀分布，突破了传统轧制压下量的限制，并可连续制备薄板类的超细晶金属材料，使得到的材料厚度较薄，同时能够能生产大块超细晶金属材料。
进一步，提供原始金属材料薄板、粗晶金属材料薄板；其中，原始金属材料薄板为提供的进行等径角挤压工艺的原始金属材料，将该原始金属材料进行线切割前处理，得到与金属材料薄板规格相同的金属材料薄板；粗晶金属材料薄板是指将原始金属材料进行粗晶化处理得到的晶粒大小更大的粗晶金属材料，该粗晶金属材料的平均晶粒尺寸没有具体的限定要求，只要达到粗晶程度即可。
进一步，提供原始金属材料薄板、粗晶金属材料薄板，与n块金属材料薄板按照晶粒尺寸的大小依次层叠设置，采用累积叠轧焊工艺依次进行叠轧处理，制备得到梯度纳米结构金属材料。将薄板按照晶粒尺寸由小到大的顺序依次层叠设置，并采用累积叠轧焊工艺依次进行叠轧处理。
在一些实施例中，根据薄板数量的不同，进而确定累积叠轧焊工艺进行叠轧处理的道次，其中，叠轧处理的道次选自但不限于3次、4次、5次。随着叠轧道次的增加，材料的抗拉强度增加；若叠轧处理的道次过多，则会随着叠轧道次的增加，氧化物夹杂物增加，结合面缺陷增加，从而降低了材料的强度；且，随着叠轧道次的增加，材料出现无屈服断裂的情况，延伸率呈下降趋势。
在具体实施例中，当原始金属材料薄板、粗晶金属材料薄板，与3块不同晶粒尺寸的金属材料薄板按照晶粒尺寸的大小依次层叠设置，采用累积叠轧焊工艺依次进行叠轧处理包括：将第一层金属材料薄板和第二层金属材料薄板进行叠轧处理形成第一复合金属材料；将第一复合金属材料和第三金属材料薄板进行叠轧处理形成第二复合金属材料；将第二复合金属材料和第四金属材料薄板进行叠轧处理形成第三复合金属材料；将第三复合金属材料和第五金属材料薄板进行叠轧处理形成梯度纳米结构金属材料。
在一些实施例中，采用累积叠轧焊工艺依次进行叠轧处理的步骤中，包括：提供两辊轧机，在最大轧制力为200~250 t，轧制速度0.5~1.0 m/s的条件下进行叠轧处理，其中，两辊轧机的辊子直径为230~250 mm，辊子长度为200~250 mm。控制叠轧处理的最大轧制力和轧制速度，能够保证得到的金属材料整体均具有梯度纳米结构，使得到的梯度纳米结构金属材料能够同时保证具有较高的材料强度以及材料韧性，以实现使用需求，扩大了使用范围。
在本发明具体实施例中，采用累积叠轧焊工艺依次进行叠轧处理的步骤中，包括：提供两辊轧机，在最大轧制力为200 t，轧制速度0.5 m/s的条件下进行叠轧处理，其中，两辊轧机的辊子直径为230 mm，辊子长度为20 mm。
本申请实施例第二方面提供一种梯度纳米结构金属材料，梯度纳米结构金属材料为块状梯度纳米结构金属材料，梯度纳米结构金属材料从表面至芯部为依次层叠设置的不同晶粒尺寸的金属材料薄板，晶粒尺寸从表面至芯部依次为从小到大的不同晶粒尺寸。
本申请第二方面提供的一种梯度纳米结构金属材料，梯度纳米结构金属材料为块状梯度纳米结构金属材料，梯度纳米结构金属材料从表面至芯部为依次层叠设置的不同晶粒尺寸的金属材料薄板，晶粒尺寸从表面至芯部依次为从小到大的不同晶粒尺寸；由于梯度纳米结构金属材料整体具有梯度纳米结构，使得到的梯度纳米结构金属材料能够同时保证具有较高的材料强度以及材料韧性，同时该梯度纳米结构金属材料的梯度纳米结构以及晶粒尺寸均可调节，得到的产品适用性广，可根据实际的需求进行设置，实现了广泛应用。
在一些实施中，梯度纳米结构金属材料的厚度为0.5~1 mm，控制得到的梯度纳米结构金属材料在较薄的结构下也具有多个梯度的纳米结构晶粒，使得到的梯度纳米结构金属材料能够同时保证具有较高的材料强度以及材料韧性。
下面结合具体实施例进行说明。
实施例1
纯铜梯度纳米结构金属材料及其制备方法
纯铜梯度纳米结构金属材料的制备方法
纯铜梯度纳米结构金属材料的制备方法包括如下步骤：
提供纯铜原始金属材料，其中，原始材料选自直径15 mm、平均晶粒大小约为7 μm的纯铜棒料；
采用等径角挤压工艺将3块纯铜棒料分别进行4个道次、6个道次、8个道次的挤压处理，得到3块不同晶粒尺寸的金属材料；其中，挤压处理的温度为室温25℃，通道相交的内模具拐角Φ为90°；通道相交的模具圆心角Ψ为90°进行等径角挤压处理。进一步的，进行4个道次挤压处理的纯铜材料的平均晶粒尺寸为0.95 μm，6个道次挤压处理的纯铜材料的平均晶粒尺寸为0.79 μm，8个道次挤压处理的纯铜材料的平均晶粒尺寸为0.51 μm；
将3块不同晶粒尺寸的金属材料采用线切割工艺分别进行切割处理，其中，线切割工艺包括：电压为70 V，电流为0.4 A，脉宽比为3：4；再进行除杂处理，除杂处理为采用1500目的砂纸进行打磨处理15分钟，采用无水乙醇进行超声清洗处理15分钟，得到3块不同晶粒尺寸的金属材料薄板，其中，金属材料薄板的厚度为长50 mm、宽10mm、厚度是1mm；
提供金属材料薄板，将纯铜原始金属材料进行线切割处理，得到厚度为长50 mm、宽10mm、厚度是1mm的金属材料薄板；
提供粗晶金属材料薄板，将纯铜原始金属材料在873 K温度下退火4 h得到晶粒尺寸是15 μm的粗晶纯铜材料，并进行线切割处理，得到厚度为长50 mm、宽10mm、厚度是1mm的粗晶金属材料薄板；
将平均晶粒尺寸为0.51 μm的金属材料薄板与平均晶粒尺寸为0.79 μm的金属材料薄板依次进行层叠设置，进行第一道叠轧工艺处理形成第一复合金属材料；将第一复合金属材料与平均晶粒尺寸为0.95 μm的金属材料薄板依次进行层叠设置，进行第二道叠轧工艺处理形成第二复合金属材料；将第二复合金属材料与金属材料薄板依次进行层叠设置，进行第三道叠轧工艺处理形成第三复合金属材料；将第三复合金属材料与粗晶金属材料薄板依次层叠设置，进行第四道叠轧工艺处理形成梯度纳米结构金属材料；其中，进行叠轧处理的步骤中，包括：提供两辊轧机，在最大轧制力为200 t，轧制速度0.5 m/s的条件下进行叠轧处理，其中，两辊轧机的辊子直径为230 mm，辊子长度为200 mm。
纯铜梯度纳米结构金属材料
梯度纳米结构金属材料为块状梯度纳米结构金属材料，梯度纳米结构金属材料从表面至芯部为依次层叠设置的不同晶粒尺寸的金属材料薄板，且，晶粒尺寸从表面至芯部依次为0.51微米、0.79微米、0.95微米、7微米、15微米。
实施例2
6061铝合金梯度纳米结构金属材料及其制备方法
6061 铝合金梯度纳米结构金属材料的制备方法
6061铝合金梯度纳米结构金属材料的制备方法包括如下步骤：
提供6061铝合金原始金属材料，其中，原始材料选自直径15 mm、平均晶粒大小约为7 μm的纯铜棒料；
采用等径角挤压工艺将3块6061铝合金棒料分别进行4个道次、6个道次、8个道次的挤压处理，得到3块不同晶粒尺寸的金属材料；其中，挤压处理的温度为室温25℃，通道相交的内模具拐角Φ为90°；通道相交的模具圆心角Ψ为90°进行等径角挤压处理。进一步的，进行4个道次挤压处理的6061铝合金材料的平均晶粒尺寸为0.8 μm，6个道次挤压处理的6061铝合金材料的平均晶粒尺寸为0.7 μm，8个道次挤压处理的6061铝合金材料的平均晶粒尺寸为0.45 μm；
将3块不同晶粒尺寸的金属材料采用线切割工艺分别进行切割处理，其中，线切割工艺包括：电压为70 V，电流为0.4 A，脉宽比为3：4；再进行除杂处理，除杂处理为采用1500目的砂纸进行打磨处理15分钟，采用无水乙醇进行超声清洗处理15分钟，得到3块不同晶粒尺寸的金属材料薄板，其中，金属材料薄板的厚度为长50 mm、宽10mm、厚度是1mm；
提供金属材料薄板，将6061铝合金原始金属材料进行线切割处理，得到厚度为长50 mm、宽10mm、厚度是1mm的金属材料薄板；
提供粗晶金属材料薄板，提供晶粒尺寸为20 μm的6061铝合金，并进行线切割处理，得到厚度为长50 mm、宽10mm、厚度是1mm的粗晶金属材料薄板；
将平均晶粒尺寸为0.45 μm的金属材料薄板与平均晶粒尺寸为0.7 μm的金属材料薄板依次进行层叠设置，进行第一道叠轧工艺处理形成第一复合金属材料；将第一复合金属材料与平均晶粒尺寸为0.8 μm的金属材料薄板依次进行层叠设置，进行第二道叠轧工艺处理形成第二复合金属材料；将第二复合金属材料与金属材料薄板依次进行层叠设置，进行第三道叠轧工艺处理形成第三复合金属材料；将第三复合金属材料与粗晶金属材料薄板依次层叠设置，进行第四道叠轧工艺处理形成梯度纳米结构金属材料；其中，进行叠轧处理的步骤中，包括：提供两辊轧机，在最大轧制力为200 t，轧制速度0.5 m/s的条件下进行叠轧处理，其中，两辊轧机的辊子直径为230 mm，辊子长度为200 mm。
6061 铝合金梯度纳米结构金属材料
梯度纳米结构金属材料为块状梯度纳米结构金属材料，梯度纳米结构金属材料从表面至芯部为依次层叠设置的不同晶粒尺寸的金属材料薄板，且，晶粒尺寸从表面至芯部依次为0.45微米、0.7微米、0.8微米、7微米、20微米。
性能测试和结果分析：
将实施例1分别进行4个道次、6个道次、8个道次的等径角挤压工艺处理得到的纯铜金属材料的微结构进行EBSD表征，其中，进行4个道次的等径角挤压工艺处理得到的纯铜金属材料如附图5所示，平均晶粒尺寸为0.95微米；进行6个道次的等径角挤压工艺处理得到的纯铜金属材料如附图6所示，平均晶粒尺寸为0.79微米；进行8个道次的等径角挤压工艺处理得到的纯铜金属材料如附图7所示，平均晶粒尺寸为0.51微米。
实施例1纯铜梯度纳米结构金属材料如附图8所示，梯度纳米结构金属材料从表面至芯部为依次层叠设置的不同晶粒尺寸的金属材料薄板，且，晶粒尺寸从表面至芯部依次为0.51微米、0.79微米、0.95微米、7微米、15微米。
将实施例2分别进行4个道次、6个道次、8个道次的等径角挤压工艺处理得到的6061铝合金金属材料的微结构进行EBSD表征，其中，进行4个道次的等径角挤压工艺处理得到的6061铝合金金属材料如附图9所示，平均晶粒尺寸为0.8微米；进行6个道次的等径角挤压工艺处理得到的6061铝合金金属材料如附图10所示，平均晶粒尺寸为0.7微米；进行8个道次的等径角挤压工艺处理得到的6061铝合金金属材料如附图11所示，平均晶粒尺寸为0.45微米。
实施例2 6061铝合金梯度纳米结构金属材料如附图12所示，梯度纳米结构金属材料从表面至芯部为依次层叠设置的不同晶粒尺寸的金属材料薄板，且，晶粒尺寸从表面至芯部依次为0.45微米、0.7微米、0.8微米、7微米、20微米。
将实施例1和实施例2制备得到的梯度纳米结构金属材料的硬度和延伸率分别进行测试，其中，实施例1得到的纯铜梯度纳米结构金属材料的上表层显微硬度约HV130，而最下层的显微硬度约HV70；拉伸测试显示，制备的纯铜梯度纳米结构金属材料的延伸率明显高于超细晶材料而接近粗晶材料的延伸率；实施例2得到的6061铝合金梯度纳米结构金属材料的上表层显微硬度约HV100，而最下层的显微硬度约HV60；拉伸测试显示，制备的纯铜梯度纳米结构金属材料的延伸率明显高于超细晶材料而接近粗晶材料的延伸率。
综上，提供的梯度纳米结构金属材料的制备方法，该制备方法先采用等径角挤压工艺将金属材料进行反复挤压若干道次后获得具有不同晶粒尺寸的金属材料，通过控制挤压得道次不同，可以控制得到得晶粒尺寸的大小，可根据需要进行调整；再经过线切割处理，得到大小一致的不同晶粒尺寸的金属材料薄片，再利用累积叠轧焊的方法依次将两块大小一致的金属材料薄片进行轧制，循环反复几次后就可以把薄片叠轧焊和，得到具有梯度纳米结构的金属材料，与现有技术中距离表面一小段距离具有梯度纳米结构的金属材料相比，该制备方法是基于等径角挤压和累积叠轧焊工艺，采用两种方法协同作用得到的金属材料整体均具有梯度纳米结构，可根据实际需要，控制得到的金属材料具有不同的梯度纳米结构，同时也可对晶粒尺寸的大小进行控制，因此，该制备方法简便易操作，灵活性大，可根据实际需求，进一步对金属材料的梯度纳米结构以及晶粒尺寸大小进行控制，使得到的梯度纳米结构金属材料能够同时保证具有较高的材料强度以及材料韧性，以实现使用需求，扩大了使用范围。
以上仅为本申请的较佳实施例而已，并不用以限制本申请，凡在本申请的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本申请的保护范围之内。

Claims (10)

  1. 一种梯度纳米结构金属材料的制备方法，其特征在于，包括如下步骤：
    提供n块原始金属材料，采用等径角挤压工艺将所述原始金属材料分别进行不同道次的挤压处理，得到n块具有不同晶粒尺寸的金属材料，其中，n不少于3；
    将n块所述金属材料采用线切割工艺分别进行切割处理，并进行除杂处理，得到n块具有不同晶粒尺寸的金属材料薄板；
    提供原始金属材料薄板、粗晶金属材料薄板，与n块所述金属材料薄板按照晶粒尺寸的大小依次层叠设置，采用累积叠轧焊工艺依次进行叠轧处理，制备得到梯度纳米结构金属材料。
  2. 根据权利要求1所述的梯度纳米结构金属材料的制备方法，其特征在于，所述等径角挤压工艺的模具为由两个具有相同形状且横截面积相等的通道按照一定的角度相互交截组成的，两通道相交的内模具拐角为Φ，通道相交的模具圆心角为Ψ，所述通道相交的内模具拐角为Φ，90°≤Φ≤120°；所述通道相交的模具圆心角等于Ψ，且60°≤Ψ≤90°。
  3. 根据权利要求1所述的梯度纳米结构金属材料的制备方法，其特征在于，采用等径角挤压工艺将所述原始金属材料分别进行不同道次的挤压处理的步骤中，分别进行1~8任意道次的挤压处理。
  4. 根据权利要求1~3任一所述的梯度纳米结构金属材料的制备方法，其特征在于，将n块所述金属材料采用线切割工艺分别进行切割处理的步骤中，包括：将n块所述金属材料分别垂直固定在设备上，利用线切割工艺将所述金属材料进行切割处理。
  5. 根据权利要求4所述的梯度纳米结构金属材料的制备方法，其特征在于，所述线切割工艺包括：电压为70~75 V，电流为0.4~0.5 A，脉宽比为（3~3.5）：4。
  6. 根据权利要求1~3任一所述的梯度纳米结构金属材料的制备方法，其特征在于，除杂处理包括：采用砂纸进行打磨处理，采用有机溶剂进行超声清洗处理。
  7. 根据权利要求6所述的梯度纳米结构金属材料的制备方法，其特征在于，所述打磨处理的时间为15~20分钟；和/或，
    所述超声清洗处理的时间为10~15分钟。
  8. 根据权利要求1~3任一所述的梯度纳米结构金属材料的制备方法，其特征在于，所述金属材料薄板的长度为50~100 mm，宽度为10~20 mm，厚度为0.5~1 mm。
  9. 根据权利要求1~3任一所述的梯度纳米结构金属材料的制备方法，其特征在于，采用累积叠轧焊工艺依次进行叠轧处理的步骤中，包括：提供两辊轧机，在最大轧制力为200~250 t，轧制速度0.5~1.0 m/s的条件下进行叠轧处理，其中，所述两辊轧机的辊子直径为230~250 mm，辊子长度为200~250 mm。
  10. 一种梯度纳米结构金属材料，其特征在于，所述梯度纳米结构金属材料为块状梯度纳米结构金属材料，所述梯度纳米结构金属材料从表面至芯部为依次层叠设置的不同晶粒尺寸的金属材料薄板，且，所述晶粒尺寸从表面至芯部依次为从小到大的不同晶粒尺寸。
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