CN111621670B - Multi-grain-size core-shell-structure titanium alloy block material and preparation method thereof - Google Patents
Multi-grain-size core-shell-structure titanium alloy block material and preparation method thereof Download PDFInfo
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- CN111621670B CN111621670B CN202010581793.6A CN202010581793A CN111621670B CN 111621670 B CN111621670 B CN 111621670B CN 202010581793 A CN202010581793 A CN 202010581793A CN 111621670 B CN111621670 B CN 111621670B
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- 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
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Abstract
The invention discloses a multi-grain-scale core-shell structure titanium alloy block material and a preparation method thereof, and relates to the field of powder metallurgy. The preparation method comprises the following steps: putting the raw materials into a ball milling tank, uniformly mixing, and then carrying out high-energy ball milling to obtain nanocrystalline mixed powder; pressing the nanocrystalline mixed powder into a green body; heating the green body to raise the temperature; moving the heated green body into a preheated extrusion die, and carrying out hot extrusion to obtain a titanium alloy bar; and cooling to room temperature to obtain the multi-grain-size core-shell structure titanium alloy block material. The multi-grain-size core-shell structure titanium alloy block material provided by the invention has the advantages of high strength and high work hardening capacity; the preparation method greatly reduces the cost of raw materials, has simple process flow and has the potential of large-scale production.
Description
Technical Field
The invention relates to the field of powder metallurgy, in particular to a multi-grain-size core-shell structure titanium alloy block material and a preparation method thereof.
Background
Titanium alloy is an important nonferrous metal material, has excellent physicochemical properties such as small density, high specific strength and specific modulus, good plasticity and toughness, strong corrosion resistance, good biocompatibility and wide use temperature range, plays a role of a key structural part in a plurality of important fields such as military industry, automobile industry, aerospace, chemical industry, biomedical treatment and the like, and is called as 'metal in the 21 st century' and 'third metal which is rising'.
In the automobile industry, safety, energy conservation and environmental protection become three main subjects of industry development, the reduction of fuel consumption and the reduction of emission of CO, inhalable particles and other toxic gases become very important development directions, and therefore the requirement for realizing the light weight of automobiles is increasing day by day; with the development of the aerospace industry, a more severe working environment puts higher requirements on realizing the weight reduction and performance improvement of the structure of the spacecraft, so that structural materials with higher specific strength and higher specific modulus need to be developed. In common metal structural materials, the titanium alloy has the highest specific strength, so that the prepared titanium alloy with higher strength can further explore the application potential of titanium in the fields of automobiles, aviation and the like.
The preparation of ultra-fine grain and nano-grain metal materials is a classic method for strengthening metal structural materials by reducing the grain size of the metal materials. However, these structures, while increasing the strength of the metal material, generally significantly reduce the plasticity and work hardening capabilities of the metal material. For example, R.S.Mishra et Al (R.S.Mishra, V.V.Stolyarov, C.Echer, R.Z.Valiev, A.K.Mukherjee, Materials Science and Engineering A298, (2001)44-50) prepared nanocrystalline Ti-6Al-4V disk samples from commercial Ti-6Al-4V alloys by high pressure torsion process, the Materials achieved tensile yield strength and tensile strength of 1275MPa and 1418MPa respectively, however, elongation was only 1.2%, and such low tensile elongation severely compromised the service safety of the metallic Materials. Therefore, the improvement of the plasticity of the high-strength titanium alloy has great scientific and engineering significance.
By adding the coarse crystals with proper volume fraction into the ultrafine crystal or nano crystal structure, the bimodal or multimodal distribution of the grain size can be realized, so that the material has both the high strength of the nano crystals and the high plasticity of the coarse crystals, and the plasticity of the ultrafine crystal matrix is improved at the expense of partial strength. In recent years, researchers find that the comprehensive performance of the material can be further improved by controlling the distribution of the coarse and fine grain regions through structural design, and better strong/plastic matching is realized.
The core-shell structure is an organization structure with special distribution of coarse and fine crystal regions, and the concept was introduced into the field of metal structure Materials by the professor of Japanese Kei Ameryama (Sanjay Kumar Vajpai, Mie Ota, Zhe Zhang, Kei Ameryama, Materials Research Letters 4, (2016) 191-197). At present, the characteristics of the core-shell structure model reported in the literature can be summarized as that fine crystal areas form a three-dimensional net-shaped framework, and coarse crystal areas are filled in the framework. For example, Vajpai et Al (S.K. Vajpai, M.Ota, T.Watanabe, R.Maeda, T.Sekiguchi, T.Kusaka, K.Ameyama, Metallurgical and Materials transformations A46, (2015)903-914) prepared core-shell Ti-6Al-4V alloys, the coarse nuclei of which were composed of (α -Ti + β -Ti) sheets and the fine shells of which were composed of α -Ti equiaxed grains, the tensile yield strength and tensile strength of which were 915MPa and 956MPa, respectively, with elongations as high as 22%.
At present, the processes for preparing the core-shell structure reported in the literature all utilize low-energy ball milling and subsequent thermal consolidation processes to treat spherical powder. The low-energy ball milling enables the surface of powder particles to be impacted by the grinding balls to form a fine-grain region, while coarse-grain morphology is still kept inside the powder particles, so that the spherical powder forms a special organization structure of a fine-grain shell wrapping coarse crystal nucleus; and then, the special structure of the powder particles is kept through rapid thermal consolidation processes such as spark plasma sintering and the like, so that the fully-compact core-shell structure block material can be prepared.
In conclusion, the metals for preparing the core-shell structure titanium alloy block material at present have the following defects:
(1) the titanium or titanium alloy powder has stronger ductility, and is easy to generate cold welding phenomenon in the ball milling process and adhere to the wall of the tank or the grinding ball, so that the powder refining efficiency is low, and the powder yield is low;
(2) the cost of the titanium alloy spherical powder raw material is too high, for example, the price of Ti-6Al-4V spherical powder with better quality is generally more than 2000 yuan/kg;
(3) the low energy ball milling introduces low energy, has limited degree of refining the powder particles, is generally difficult to refine the grains on the surface of the powder particles to the size of ultrafine grains, and has small volume fraction of the fine grain area, resulting in limited improvement of the strength of the block material.
Therefore, the technical personnel in the field are dedicated to develop a multi-grain-scale core-shell structure titanium alloy block material with high strength and good plasticity, and the preparation method is simpler in process, low in cost and easy to scale.
Disclosure of Invention
In view of the above defects in the prior art, the technical problem to be solved by the present invention is how to provide a multi-grain-size core-shell structure titanium alloy block material with high strength and good plasticity, and the preparation method has the advantages of simpler process, low cost and easy scale production.
In order to achieve the purpose, the invention provides a multi-grain-size core-shell structure titanium alloy block material, wherein the core-shell structure is formed by wrapping a coarse-grain slice layer with an ultrafine-grain slice layer, the coarse-grain slice layer is a coarse-grain alpha-Ti slice layer, and the ultrafine-grain slice layer is an (alpha-Ti + beta-Ti + delta-TiH) slice layer.
Further, the thickness of the coarse wafer layer is 1-2 μm, the thickness of the superfine wafer layer is 50-250 nm, and the average size of the unit body of the core-shell structure is 10 μm.
The invention also provides a preparation method of the multi-grain-size core-shell structure titanium alloy block material, which comprises the following steps:
and 5, cooling the titanium alloy bar obtained in the step 4 to room temperature to obtain the titanium alloy block material with the multi-grain-size core-shell structure.
Furthermore, the whole process of the preparation method is carried out in a closed system isolated from the atmosphere, that is, the ball milling tank in the step 1 and the operation box in the step 2 can be vacuumized and filled with argon gas, so that the oxygen content is always lower than 200 ppm.
Further, the raw materials in the step 1 are titanium hydride and master alloy raw materials, wherein the master alloy raw materials are master alloy particles or powder capable of performing an alloying reaction with titanium to generate a titanium alloy with a required composition.
Further, the low energy ball milling and the high energy ball milling in the step 1 may be performed using a planetary ball mill, an agitator ball mill, or a drum ball mill; wherein the technological parameters of the low-energy ball milling are as follows: the mass ratio of the grinding balls to the raw materials is 1: 1-50: 1, the ball milling rotation speed is 50-300 rpm, and the ball milling time is 0.5-12 hours; the technological parameters of the high-energy ball milling are as follows: the mass ratio of the grinding balls to the raw materials is 1: 1-50: 1, the ball milling rotation speed is 400-500 rpm, and the ball milling time is 1-12 hours.
Further, the parameters of the molding in the step 2 are as follows: the applied pressure is 500-1500 MPa, and the pressure maintaining time is 1-10 minutes.
Further, the heating temperature rise in the step 3 can be realized by induction heating or microwave heating; the temperature range of heating and temperature rise is 1000-1200 ℃, the temperature rise rate is 50-200 ℃/min, and the heat preservation time is 2-10 min.
Further, the parameters of the hot extrusion in the step 4 are set as follows: the preheating temperature is 400-500 ℃, the pressure is 800-1500 MPa, and the extrusion ratio is 5: 1-50: 1.
Further, the cooling in step 5 may be performed by air cooling, oil quenching or water quenching.
Compared with the prior art, the invention at least has the following beneficial technical effects:
(1) the invention adopts titanium hydride and other intermediate alloy powder or particles as raw materials, and the cost is obviously lower than that of titanium alloy spherical powder;
(2) because the titanium hydride and other intermediate alloys are very brittle in nature and have high grain refinement efficiency, the titanium hydride and other intermediate alloys can be refined to a nanometer level through short-time high-energy ball milling, and the powder yield is extremely high and is close to 100%;
(3) the invention adopts rapid heating modes such as induction heating and the like, reduces the retention time of the blank at high temperature, thereby inhibiting the growth of crystal grains of the blank in the heating and hot extrusion processes, keeping the fine crystal structure obtained by ball milling as much as possible, ensuring that most areas in the block material are fine crystal lamella layers and having more obvious fine crystal strengthening effect;
(4) the process combining the high-energy ball milling and the thermal mechanical consolidation can utilize the existing equipment of the oxide dispersion strengthening high-temperature alloy preparation process, and is easy to realize large-scale industrial production;
(5) by adjusting the technological parameters such as ball milling time, heating rate, heat preservation temperature, cooling rate and the like, the invention can flexibly adjust the size and volume ratio of coarse and fine grain regions in the microstructure, and realize the adjustment of the strength and plasticity of the block material in a certain range.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
FIG. 1 is a SEM backscatter image of a microstructure of a multi-grain-scale core-shell Ti-6Al-4V alloy rod prepared according to a preferred embodiment of the invention;
FIG. 2 is an XRD contrast diagram of a multi-grain-size core-shell Ti-6Al-4V alloy rod prepared by a preferred embodiment of the invention and high-energy ball-milled powder;
FIG. 3 is a room temperature tensile engineering stress-strain curve of a multi-grain-scale core-shell Ti-6Al-4V alloy rod prepared according to a preferred embodiment of the present invention.
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
In the embodiment, a multi-grain-size core-shell-structured Ti-6Al-4V alloy rod is prepared by the following steps:
and 6, closing the heating coil of the die, placing the extruded Ti-6Al-4V bar in an argon atmosphere for air cooling to room temperature, and then taking out to obtain the Ti-6Al-4V extrusion bar.
A scanning electron microscope is used for representing the Ti-6Al-4V extrusion rod obtained in the embodiment, and an obtained electron microscope photo is shown in figure 1, so that the structural structure of the extrusion rod is proved to be the characteristic of a multi-grain-size core-shell structure of a coarse-grain sheet layer wrapping a fine-grain sheet layer.
The steps described in this example2 obtaining the nanocrystalline TiH2/Al60V40XRD analysis of the mixed powder and the Ti-6Al-4V extruded rod obtained in the step 6 is carried out, and the result is shown in figure 2, and the XRD pattern obtained by comparison analysis shows that the Ti-6Al-4V extruded rod is completely alloyed and is substantially completely dehydrogenated.
The room temperature tensile curve of the Ti-6Al-4V extrusion rod obtained in the embodiment is shown in FIG. 3, the yield strength of the sample is 1308MPa, the tensile strength is 1555MPa, the elongation is 3.5%, the strength of the sample exceeds that of a common titanium alloy-based composite material, and the sample has good work hardening capacity.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. The titanium alloy block material with the multi-grain-size core-shell structure is characterized in that the core-shell structure is formed by wrapping a coarse-grain slice layer with an ultrafine-grain slice layer, wherein the coarse-grain slice layer is a coarse-grain alpha-Ti slice layer, and the ultrafine-grain slice layer is an (alpha-Ti + beta-Ti + delta-TiH) slice layer.
2. The multi-grain-size core-shell structure titanium alloy block material according to claim 1, wherein the thickness of the coarse wafer layer is 1-2 μm, the thickness of the ultrafine wafer layer is 50-250 nm, and the average size of the unit bodies of the core-shell structure is 10 μm.
3. The preparation method of the multi-grain-size core-shell-structure titanium alloy block material according to any one of claims 1 to 2, wherein the method comprises the following steps:
step 1, putting a titanium hydride raw material and a master alloy raw material into a ball milling tank provided with milling balls, uniformly mixing the raw materials through low-energy ball milling, and then performing high-energy ball milling to obtain nanocrystalline mixed powder;
step 2, after the ball milling tank is placed in an operation box, taking out the nanocrystalline mixed powder obtained in the step 1 and preparing a green body through mould pressing;
step 3, heating the green body obtained in the step 2 to remove hydrogen in the green body;
step 4, moving the heated green body into a preheated extrusion die, and carrying out hot extrusion to obtain a titanium alloy bar;
and 5, cooling the titanium alloy bar obtained in the step 4 to room temperature to obtain the titanium alloy block material with the multi-grain-size core-shell structure.
4. The method for preparing the titanium alloy block material with the multi-grain-size core-shell structure according to claim 3, wherein the whole process of the preparation method is performed in a closed system isolated from the atmosphere, that is, the ball milling tank in the step 1 and the operation box in the step 2 can be vacuumized and filled with argon gas, so that the oxygen content is always lower than 200 ppm.
5. The method for preparing a titanium alloy block material with a multi-grain-size core-shell structure according to claim 3, wherein the titanium hydride raw material in the step 1 comprises titanium hydride powder or particles, and the master alloy raw material is master alloy particles or powder of a titanium alloy capable of performing an alloying reaction with titanium to generate a desired composition.
6. The method for preparing a titanium alloy block material with a multi-grain-size core-shell structure according to claim 3, wherein the low-energy ball milling and the high-energy ball milling in step 1 are performed by a planetary ball mill, a stirred ball mill or a roller ball mill; wherein the technological parameters of the low-energy ball milling are as follows: the mass ratio of the grinding balls to the raw materials is 1: 1-50: 1, the ball milling rotation speed is 50-300 rpm, and the ball milling time is 0.5-12 hours; the technological parameters of the high-energy ball milling are as follows: the mass ratio of the grinding balls to the raw materials is 1: 1-50: 1, the ball milling rotation speed is 400-500 rpm, and the ball milling time is 1-12 hours.
7. The method for preparing the titanium alloy block material with the multi-grain-size core-shell structure according to claim 3, wherein the die pressing parameters in the step 2 are as follows: the applied pressure is 500-1500 MPa, and the pressure maintaining time is 1-10 minutes.
8. The method for preparing the multi-grain-size core-shell-structure titanium alloy block material according to claim 3, wherein the heating and temperature rise in the step 3 can be realized by induction heating or microwave heating; the temperature range of heating and temperature rise is 1000-1200 ℃, the temperature rise rate is 50-200 ℃/min, and the heat preservation time is 2-10 min.
9. The method for preparing a multi-grain-size core-shell-structure titanium alloy block material according to claim 3, wherein the parameters of the hot extrusion in the step 4 are set as follows: the preheating temperature is 400-500 ℃, the pressure is 800-1500 MPa, and the extrusion ratio is 5: 1-50: 1.
10. The method for preparing the multi-grain-size core-shell-structure titanium alloy block material according to claim 3, wherein the cooling in the step 5 is performed by air cooling, oil quenching or water quenching.
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| CN114032409B (en) * | 2021-11-11 | 2022-09-02 | 西北工业大学 | Preparation method of low-cost high-performance titanium-oxygen alloy material |
| CN114058901B (en) * | 2021-11-16 | 2022-08-23 | 东北大学 | Submicron yttrium oxide particle toughened high-performance near-alpha powder metallurgy titanium alloy and preparation method thereof |
| CN114752874B (en) * | 2022-03-25 | 2023-04-14 | 重庆大学 | Multi-scale structure for synergistically optimizing strong plasticity of TA19 titanium alloy and preparation method thereof |
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