CN111251691A - Preparation method of multi-scale structure titanium alloy material - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/043—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
- B32B37/1018—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure using only vacuum
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- 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
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- 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
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
Abstract
The invention discloses a preparation method of a multi-scale structure titanium alloy material, belonging to the technical field of material preparation, and the technical scheme of the method is as follows: (1) pretreating a titanium plate; (2) stacking: stacking the titanium plates with different thicknesses processed in the step (1) according to a certain sequence; (3) vacuum hot-pressing sintering; (4) and (4) rolling at low temperature. According to the invention, the multi-scale titanium alloy material with adjustable structure and excellent comprehensive mechanical property can be prepared by adjusting the lamination design mode of the titanium alloy, the vacuum heat treatment and hot-pressing sintering parameters and the rolling process.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a preparation method of a multi-scale structure titanium alloy material.
Background
The titanium alloy has the advantages of low density, high specific strength and specific modulus, good corrosion resistance and the like, and is widely applied to the aerospace and automobile industries at present. However, with the rapid development of aerospace and high-performance automobiles, the service conditions of titanium alloy parts are more severe: not only is the strength requirement of titanium alloy continuously increased, but also the toughness (plasticity) of the titanium alloy is also required to be higher, namely, the titanium alloy is required to maintain enough toughness (plasticity) while the strength of the titanium alloy is greatly increased. In general, the strength of a metal material can be significantly improved by refining grains, and the strength of a metal material having a nano-grain size can be several times that of a conventional coarse-grained (grain size is several micrometers to several hundred micrometers) metal material, but the plasticity thereof is much lower than that of the coarse-grained metal material due to its low work hardening capacity.
The multi-scale structure titanium alloy refers to a gradient crystal grain structure in which crystal grains of the titanium alloy are in gradient change from a core nanometer scale to a surface micrometer scale, or a micro-nano laminated structure in which micrometer coarse crystals and nanometer fine crystals are alternately laminated. The violent plastic deformation can refine grains, and the grains can be refined to submicron or even nanometer by controlling the plastic deformation condition. In order to obtain a gradient-structured metal material, a gradient plastic deformation is generally adopted, so that the deformation amount, the deformation rate and the like are changed in a gradient manner from the center to the surface, and a gradient structure is formed. The main preparation method comprises a surface press-in type gradient deformation method, an asynchronous rolling method and the like. The surface pressing type gradient deformation is that a hard pressure head or a ball is pressed on the surface of a material repeatedly for multiple times in a circulating mode, so that the surface of the material generates repeated plastic deformation for multiple times, and the deformation quantity and the deformation rate are reduced in a gradient mode along with the increase of the depth, and a surface gradient grain structure is formed. However, the method has the limitation that the gradient structure is generated only in the depth of tens of microns on the surface of the material, and the equipment is complex and high in cost. The asynchronous rolling method is characterized in that different deformation quantities and deformation rates are generated by controlling different rolling speeds of two rollers, and plates are alternately conveyed to and fro at the same time to obtain a structure with uneven grain sizes. However, the method has extremely high requirements on the rolling mill, and the thickness of the finally rolled plate is only hundreds of microns, so that the method is not suitable for large-scale production.
Disclosure of Invention
In order to solve the problem of inversion of strength-toughness (plasticity) of the titanium alloy, the invention provides a preparation method of a multi-scale structure titanium alloy material, which adopts the following technical scheme:
a preparation method of a multi-scale structure titanium alloy material comprises the following steps:
(1) pretreating a titanium plate; (2) stacking: stacking the titanium plates with different thicknesses processed in the step (1) according to a certain sequence; (3) vacuum hot-pressing sintering; (4) and (4) rolling at low temperature.
The method comprises the following steps of utilizing a vacuum hot-pressing sintering technology to realize the interlayer preliminary combination of titanium plates with different thicknesses, and simultaneously controlling the coarsening degree of crystal grains in the titanium plates with different thicknesses (namely, the thicker the titanium plate is, the larger the size of the crystal grains is); and (3) low-temperature rolling: the method aims to realize grain refinement in titanium plates with different thicknesses, greatly improve the interlayer interface bonding strength of the titanium plates with different thicknesses, and finally prepare the titanium alloy with unevenly distributed micro-nano grains (gradient or layered distribution), namely the multi-scale structural titanium alloy block material.
The titanium plate in the step (1) is a commercial pure titanium plate, and the thickness of the titanium plate is 50 mu m-2 mm.
The step (1) is specifically as follows: the commercial pure titanium plate with the thickness of 1-2mm is firstly subjected to vacuum heat treatment, and then the surface acid treatment is carried out on the titanium plates with all specifications (the thickness is 50 mu m-2 mm).
The surface acid treatment comprises the following steps: the titanium plate is impregnated with an acid solution, rinsed with deionized water and dried.
The acid solution is hydrofluoric acid (HF) water solution with the mass concentration of 10-20%, and the dipping time is 5-30 s.
The vacuum heat treatment is carried out at the heat treatment temperature of 600-850 ℃ for 1-5 h. The heat treatment is performed in a vacuum atmosphere produced in a vacuum furnace.
The acid treatment is intended to remove impurities such as an oxide film. The deionized water rinsing can be carried out for a plurality of times, and the acid on the surface of the titanium plate is cleaned.
The vacuum heat treatment is substantially annealing treatment, and the step coarsens the crystal grains of the titanium plate to 50-200 μm.
And (3) stacking, wherein the stacking sequence is designed according to the structure of the titanium alloy material to be prepared, the larger the thickness of the titanium plate is, the larger the grain size (the coarser the grain) corresponding to the position of the prepared titanium alloy material is, and similarly, the smaller the thickness of the titanium plate is, the smaller the grain size (the finer the grain) corresponding to the position of the prepared titanium alloy material is. The method mainly comprises two laminated stacking structure designs: (a) gradient structure: placing a titanium plate with the thickness of more than or equal to 2mm in the middle, symmetrically placing titanium plates with the thickness of 1mm-50 mu m with the same thickness on two sides in sequence, and reducing the thickness of the titanium plates from the center to two sides in sequence so as to obtain a titanium alloy material with gradient grain distribution of core coarse grains and edge fine grains; (b) layered structure: the thick titanium plate with the thickness of 0.5-2mm and the thin titanium plate with the thickness of 50-100 μm are alternately arranged into a sandwich laminated structure, so as to obtain a laminated structure with coarse grains and fine grains alternately arranged, and the stacking schematic diagram of the two laminated structures is shown in figure 2.
And (3) carrying out vacuum hot-pressing sintering at the sintering temperature of 550-800 ℃, under the pressure of 20-100MPa and for the heat preservation time of 0.5-5 h.
The hot-pressing sintering realizes the interlayer primary combination of the titanium plates with different thicknesses, namely, a multilayer titanium alloy block material is obtained, and the sizes of crystal grains in the titanium plates with different thicknesses are regulated and controlled simultaneously (namely, the thicker the original titanium plate is, the bigger the crystal grains in the layer are).
And (4) rolling at low temperature of 300-700 ℃, at the rolling speed of 0.15-0.3m/s, at the total rolling deformation of 50-96%, at the first pass deformation of 20-65% and at the rest passes deformation of 5-20%, for 3-10 passes in total.
And the step of low-temperature rolling further improves the interlayer interface bonding strength of the titanium plates with different thicknesses and simultaneously regulates and controls the sizes of crystal grains in the titanium plates with different thicknesses.
Advantageous effects
According to different lamination stacking modes (see figure 2), a hot-pressing sintering technology is combined to carry out structural design on the titanium alloy, a gradient grain structure with coarse grains at the center and fine grains at the edge can be obtained, or a layered structure with the coarse grains and the fine grains arranged alternately can be obtained, then a low-temperature rolling technology is utilized to enable the material to generate violent plastic deformation, the grains in the titanium plates with different thicknesses can be refined to the micron, submicron or even nanometer level, and the finally obtained coarse grains and the fine grains in the titanium alloy are in gradient distribution or lamination distribution. The method can prepare the titanium alloy with uneven grain size, can simultaneously exert the high strength of nano fine grains and the high plasticity of micron coarse grains, and further solve the problem of inversion of strength-toughness (plasticity) of the titanium alloy. In addition, the technology of laminating, stacking and low-temperature rolling has the advantages of simple equipment, easiness in operation, low cost, capability of preparing industrial large-size plates and the like.
According to the invention, the multi-scale titanium alloy material with adjustable structure and excellent comprehensive mechanical property can be prepared by adjusting the lamination design mode of the titanium alloy, the vacuum annealing and hot-pressing sintering parameters and the rolling process.
The multi-scale structure titanium alloy material prepared by the method is characterized in that the size of internal crystal grains is micro-nano scale, and the micro-nano crystal grains are distributed in a gradient or layered manner, wherein the size of the crystal grains of a coarse crystal layer is 500nm-2 mu m, and the size of the crystal grains of a fine crystal layer is 50-300 nm; the mechanical property of the multi-scale structural titanium alloy is that the multi-scale structural titanium alloy has high strength and simultaneously keeps good plasticity and toughness.
Drawings
FIG. 1 is a flow chart of a process for preparing a multi-scale structural titanium alloy;
FIG. 2. Stack design schematic: (a) gradient structure: the middle is the thickest titanium plate (coarse crystal), the equal-thickness titanium plates are sequentially and symmetrically arranged on two sides, and the thicknesses of the titanium plates from the middle to the two sides are sequentially reduced (the sizes of crystal grains are gradually reduced); (b) layered structure: the thick titanium plates (coarse grains) and the thin titanium plates (fine grains) are alternately arranged;
FIG. 3 is a photograph of an EBSD of a multi-scale structural titanium alloy: (a) (c) the edge region is fine-grained; (b) the core region is coarse-grained.
Detailed Description
Example 1
(1) Pretreatment of a titanium plate: the thickness of the titanium plate as the raw material was 50 μm, 300 μm, 1mm, and 2mm, respectively. Firstly, placing a titanium plate with the thickness of 1mm and 2mm in a vacuum heat treatment furnace for annealing treatment to coarsen the internal crystal grains to 50-200 mu m, wherein the vacuum annealing process comprises the following steps: the temperature is 750 ℃, the heat preservation time is 2 hours, and the titanium plate with the annealing state of 1mm and the titanium plate with the annealing state of 2mm are obtained after furnace cooling. Then, carrying out surface pretreatment on all specifications of titanium plates (50 microns, 300 microns, 1mm in an annealing state and 2mm in an annealing state) by using an HF solution with the mass fraction of 15% to remove oxide films and the like (soaking for 10s), and then rinsing and drying the titanium plates by using deionized water for later use;
(2) stacking: there are two main structural designs: (a) placing 1 layer of annealed 2mm thick titanium plate in the middle, and symmetrically placing 1 layer of annealed 1mm thick titanium plate, 3 layers of 300 mu m thick titanium plate and 20 layers of 5 mu m thick titanium plate on two sides in sequence to construct a crystal grain gradient distribution structure with coarse crystal grains at the center and fine crystal grains at the edges; (b) the 1 layer of annealed 1mm thick titanium plate and 20 layers of 50 μm thick titanium plate are alternately stacked to form a sandwich laminated structure, and a layered structure with coarse grains and fine grains alternately arranged is further constructed, and a schematic diagram is shown in fig. 2. All the titanium plates used in the step are titanium plates subjected to surface treatment in the step (1).
(3) Vacuum hot-pressing sintering: and (3) carrying out vacuum hot-pressing sintering on the materials in different stacking modes, preliminarily realizing interlayer combination of titanium plates with different thicknesses, and obtaining a multilayer titanium alloy block material, wherein the sintering temperature is 700 ℃, the pressure is 50MPa, and the heat preservation time is 2 h.
(4) And (3) a low-temperature rolling process: the rolling temperature is 500 ℃, the rolling speed is 0.15m/s, the first pass deformation is 60%, the rest every pass deformation is 7%, the total rolling deformation is 95%, and the total rolling time is 6. Finally preparing the multi-scale structure titanium alloy.
TABLE 1 comparison of tensile Properties of Multi-Scale Structure titanium alloys with original macrocrystalline titanium plates
Wherein EBSD of the multi-scale titanium alloy of the stacked structure design (a) is shown in FIG. 3, and FIGS. 3(a) and (c) are microstructures of the outer surface of the sample having a grain size of about 300 nm; FIG. 3(b) shows the microstructure of the core region of the sample, which has a grain size of about 500nm, and thus it can be seen that the grain size from the core to the surface exhibits a gradient change from coarse grains to fine grains. The tensile property of the multi-scale structural titanium alloy is shown in table 1, compared with the original coarse-grained plate, the tensile strength of the multi-scale structural titanium alloy reaches 786MPa, the yield strength of the multi-scale structural titanium alloy is improved to 712MPa, the yield strength of the multi-scale structural titanium alloy is respectively improved by 120% and 163%, and the elongation after fracture is still as high as 22%.
The multi-scale structure titanium alloy of the laminated stacking structure design (b) is characterized in that the microstructure of the multi-scale structure titanium alloy is a layered structure with coarse grains and fine grains which are alternately arranged, compared with the original coarse-grain plate, the tensile strength and the yield strength of the multi-scale structure titanium alloy are respectively improved by 109% and 125%, and the elongation after fracture is up to 18%.
Example 2
The difference from example 1 is that:
the acid solution in the step (1) is an HF aqueous solution with the mass concentration of 20%, and the soaking time is 5 s. And (2) carrying out vacuum heat treatment in the step (1), wherein the heat treatment temperature is 750 ℃, and the heat treatment time is 3 hours. And (3) carrying out vacuum hot-pressing sintering at the sintering temperature of 750 ℃, the pressure of 40MPa and the heat preservation time of 1 h. And (4) rolling at low temperature, wherein the temperature is 520 ℃, the rolling speed is 0.15m/s, the total rolling deformation is 90%, the first pass deformation is 50%, and the rest passes deformation is 10%, and the rolling is performed for 5 passes.
The characteristics show that the microstructure of the multi-scale structure titanium alloy of the stacked structure design (a) shows a gradient change from coarse grains to fine grains from the core to the surface. Compared with the original coarse-grained plate, the tensile strength and the yield strength of the multi-scale structural titanium alloy are respectively improved by 101% and 123%, the elongation after fracture is up to 21%, and the multi-scale structural titanium alloy keeps enough plasticity while the strength is greatly improved.
The multi-scale structure titanium alloy of the laminated stacking structure design (b) is characterized in that the microstructure of the multi-scale structure titanium alloy is a layered structure with coarse grains and fine grains which are alternately arranged, compared with the original coarse-grain plate, the tensile strength and the yield strength of the multi-scale structure titanium alloy are respectively improved by 109% and 125%, and the elongation after fracture is as high as 17%.
Example 3
The difference from example 1 is that:
the acid solution in the step (1) is an HF aqueous solution with the mass concentration of 10%, and the soaking time is 15 s. And (2) carrying out vacuum heat treatment in the step (1), wherein the heat treatment temperature is 800 ℃, and the heat treatment time is 1 h. And (3) carrying out vacuum hot-pressing sintering at 800 ℃ under the pressure of 30MPa for 1 h. And (4) rolling at low temperature, wherein the temperature is 550 ℃, the rolling speed is 0.20m/s, the total rolling deformation is 95%, the first pass deformation is 65%, and the other passes deformation is 10%, and the rolling is carried out for 4 passes.
The characteristics show that the microstructure of the multi-scale structure titanium alloy of the stacked structure design (a) shows a gradient change from coarse grains to fine grains from the core to the surface. Compared with the original coarse-grained plate, the tensile strength and the yield strength of the multi-scale structural titanium alloy are respectively improved by 109% and 133%, the elongation after fracture is up to 23%, and the multi-scale structural titanium alloy keeps enough plasticity while the strength is greatly improved.
The multi-scale structure titanium alloy of the laminated stacking structure design (b) is characterized in that the microstructure of the multi-scale structure titanium alloy is a layered structure with coarse grains and fine grains which are alternately arranged, compared with the original coarse-grain plate, the tensile strength and the yield strength of the multi-scale structure titanium alloy are respectively improved by 101% and 121%, and the elongation after fracture is up to 18%.
Claims (9)
1. A preparation method of a multi-scale structure titanium alloy material is characterized by comprising the following steps: the method comprises the following steps:
(1) pretreating a titanium plate; (2) stacking: stacking the titanium plates with different thicknesses processed in the step (1) according to a certain sequence; (3) vacuum hot-pressing sintering; (4) and (4) rolling at low temperature.
2. The method for producing a multi-scale structural titanium alloy material according to claim 1, characterized in that: and (4) rolling at the low temperature of 300-700 ℃.
3. The method for producing a multi-scale structural titanium alloy material according to claim 2, characterized in that: and (4) rolling at low temperature, wherein the rolling speed is 0.15-0.3 m/s.
4. The method for producing a multi-scale structural titanium alloy material according to claim 3, characterized in that: and (4) carrying out low-temperature rolling, wherein the total rolling deformation is 50-96%, the first pass deformation is 20-65%, the rest passes deformation is 5-20%, and the rolling is carried out for 3-10 passes.
5. The method for producing a multi-scale structural titanium alloy material according to claim 1, characterized in that: the step (1) is specifically as follows: firstly, carrying out vacuum heat treatment on a titanium plate with the thickness of 1-2mm, and then carrying out surface acid treatment on the titanium plates with all specifications; the titanium plate in the step (1) is a pure titanium plate.
6. The method for producing a multi-scale structural titanium alloy material according to claim 5, characterized in that: the surface acid treatment comprises the following steps: the titanium plate is impregnated with an acid solution, rinsed with deionized water and dried.
7. The method for producing a multi-scale structural titanium alloy material according to claim 6, characterized in that: the acid solution is an HF aqueous solution with the mass concentration of 10-20%, and the dipping time is 5-30 s.
8. The method for producing a multi-scale structural titanium alloy material according to claim 5, characterized in that: the vacuum heat treatment is carried out, the heat treatment temperature is 600-850 ℃, and the heat treatment time is 1-5 h; the heat treatment is performed in a vacuum atmosphere produced in a vacuum furnace.
9. The method for producing a multi-scale structural titanium alloy material according to claim 1, characterized in that: the vacuum hot-pressing sintering in the step (3) is carried out, wherein the sintering temperature is 550-800 ℃, the pressure is 20-100MPa, and the heat preservation time is 0.5-5 h; the method is carried out in a vacuum environment.
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Cited By (5)
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| CN112496036A (en) * | 2020-11-12 | 2021-03-16 | 太原理工大学 | Method for preparing metal gradient material by rolling |
| CN113941831A (en) * | 2021-09-23 | 2022-01-18 | 哈尔滨理工大学 | Method for rapidly preparing gradient titanium plate based on vacuum hot pressing process |
| CN114318086A (en) * | 2021-12-08 | 2022-04-12 | 南京理工大学 | Multi-grain-size 7-series aluminum alloy composite material and preparation method thereof |
| CN114540606A (en) * | 2022-03-09 | 2022-05-27 | 西部金属材料股份有限公司 | Preparation method of high-hardness titanium alloy sheet and foil |
| CN115094261A (en) * | 2022-06-27 | 2022-09-23 | 广州赛隆增材制造有限责任公司 | Coarse-grain and fine-grain composite structure titanium alloy and preparation method and application thereof |
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Application publication date: 20200609 |