CN109825785B - Preparation method of industrial pure titanium with heterogeneous layered structure - Google Patents
Preparation method of industrial pure titanium with heterogeneous layered structure Download PDFInfo
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Abstract
The invention discloses a preparation method of industrial pure titanium with a heterogeneous layered structure, and belongs to the field of manufacturing of industrial pure titanium. Firstly, carrying out homogenization annealing treatment on industrial pure titanium with the thickness of 10-15 mm to obtain a uniform structure with the average grain size of 70 mu m; then, performing 80-90% cold rolling treatment on the steel strip to form a traditional strip-shaped cold-rolled structure; and finally, carrying out incomplete recrystallization annealing treatment for 5-60 min at the temperature of 450-500 ℃ to prepare the industrial pure titanium with the heterogeneous layered structure. The mechanical experiment result shows that the industrial pure titanium with the structure has the yield strength of 550-660 MPa and the tensile strength of 630-750 MPa, and the uniform elongation rate is more than or equal to 4% and the breaking elongation rate can be more than or equal to 15%. The industrial pure titanium with the heterogeneous layered structure solves the problem of low strength of the industrial pure titanium, simultaneously has good ductility and plasticity, improves the strong plasticity matching performance of the industrial pure titanium, and is convenient for industrial application and production.
Description
Technical Field
The invention relates to the field of preparation of industrial pure titanium, in particular to a preparation method of industrial pure titanium with a heterogeneous layered structure.
Background
Titanium and its alloy have the highest specific strength in many metals because of its high strength and excellent corrosion resistance, its specific strength is 3.5 times of stainless steel, 1.3 times of aluminum alloy matrix, 1.7 times of magnesium alloy, with the development and development of titanium alloy, the application of titanium in the civil industry will increase manyfold, especially will obtain the extensive application in civil fields such as shipbuilding, automobile manufacturing, chemical industry, electron, ocean development, biomedicine, desalination of sea water, geothermal power generation, pollution discharge and corrosion prevention, etc. Compared with titanium alloy, pure titanium does not contain elements harmful to human bodies, such as Al and V, and is increasingly concerned. But the strength of the industrial pure titanium is lower than that of the titanium alloy, so that the industrial requirement is difficult to meet. Therefore, it is critical to improve the strength of the commercially pure titanium and to provide the commercially pure titanium with certain plasticity and ductility.
Severe Plastic Deformation (SPD) can effectively refine grains to achieve the effect of improving strength, and the commonly used SPD process includes High Pressure Torsion (HPT), equal channel angular Extrusion (ECAP), repeated lap rolling (ABR), and the like. These methods, while providing a large increase in the strength of commercially pure titanium, are accompanied by a reduction in ductility and work hardening rate. Therefore, improving the strong plastic match is an important issue for commercially pure titanium.
In recent years, a great deal of research shows that the non-homogenization of the metal material can effectively improve the comprehensive mechanical property of the material. The main reason that the gradient structure, the bimodal structure, the harmonic structure and the heterogeneous layered structure can improve the strong plastic matching performance of the material is that a strain gradient and a soft-hard interface are introduced into the material, the yield strength of the material is improved by refined grains and back stress in the deformation process, and meanwhile, the tensile plasticity of the material is enhanced by a large number of geometrical essential dislocations propagated at the soft-hard interface.
In the existing method, Wu et al adopt a method of combining asynchronous rolling and heat treatment to prepare the industrial pure titanium with a heterogeneous layered structure, the strength of the industrial pure titanium is close to 1000MPa at the highest, and the uniform elongation reaches 9 percent.
The traditional rolling and the subsequent incomplete recrystallization annealing treatment can effectively realize the material structure function integrated design, have universality for various conventional engineering metal materials and have very wide application prospect.
Disclosure of Invention
The invention aims to provide a preparation method of industrial pure titanium with a heterogeneous layered structure aiming at the contradiction that the strength of coarse crystalline industrial pure titanium is low and the plasticity of ultra-fine crystalline/nano crystalline industrial pure titanium is extremely low.
The technical scheme adopted for realizing the aim of the invention is as follows: a method for preparing industrial pure titanium with a heterogeneous layered structure, wherein the chemical composition (wt.%) of the industrial pure titanium is as follows: 0.15O,0.01N,0.01C,0.03Fe, and the balance Ti and inevitable impurities.
The method comprises the following specific steps:
(1) homogenizing annealing treatment
And (3) preserving the heat of the industrial pure titanium with the thickness of 10-15 mm for 2 hours at the temperature of 750 ℃ in a tubular vacuum annealing furnace to obtain a homogenized structure, wherein the average grain size of the homogenized structure is 70 microns.
(2) Cold rolling treatment
Polishing the surface of the industrial pure titanium-titanium plate subjected to the homogenizing annealing treatment by using sand paper, and then performing cold rolling treatment at room temperature, wherein the thickness of the original plate is 10-15 mm, the thickness of the rolled plate is 1-3 mm, the rolling amount of each pass is 0.3-0.5 mm, and the total rolling reduction is 80-90%.
(3) Annealing treatment for incomplete recrystallization
And heating the tubular vacuum annealing furnace to 450-500 ℃, moving the heat preservation box to a sample position, carrying out heat preservation annealing treatment for 5-60 min, and then cooling to room temperature in an air cooling mode.
Compared with the prior art, the invention has the following remarkable advantages:
1) the invention adopts a method of combining the synchronous cold rolling at the room temperature with the incomplete recrystallization annealing with the larger deformation to prepare the industrial pure titanium with the heterogeneous layered structure mixed with micron-sized recrystallization, ultrafine grain and cold-rolled residual elongated coarse crystal phase, and the industrial pure titanium has certain strength and good plasticity through the coordinated strain of soft phase and hard phase and the back stress strengthening, thereby finally improving the comprehensive mechanical property of the industrial pure titanium.
The mechanical tensile test result of the heterogeneous layered industrial pure titanium prepared by the method is as follows: the yield strength of the industrial pure titanium is 550-660 MPa, the tensile strength is 630-750 MPa, the uniform elongation rate can reach more than or equal to 4%, and the fracture elongation rate can reach more than or equal to 15%.
2) The cold rolling process is carried out at room temperature, synchronous rolling is adopted, and the annealing temperature is medium-low temperature (slightly low)
At the recrystallization temperature), the cost can be effectively saved by adopting medium-low temperature annealing.
3) The thickness of the titanium plate used in the invention is 10-15 mm, belongs to the conventional application size, and is suitable for industrial application. The invention has simple process conditions and simple and convenient operation, and can be applied to industrial production.
Drawings
FIG. 1 is an EBSD topography of coarse grain commercially pure titanium after a homogenizing anneal in an example;
FIG. 2 is an EBSD topography of the industrially pure titanium with a heterogeneous layered structure after the annealing treatment of cold rolling and incomplete recrystallization in the example;
FIG. 3 is a graph of engineering stress-engineering strain curves for coarse-grained commercially pure titanium and for non-homogeneous layered structure commercially pure titanium after annealing for cold rolling and incomplete recrystallization in the examples.
Detailed Description
The invention is further described in detail below with reference to the figures and the specific embodiments.
Example one
First, the present embodiment adopts the following apparatus:
hot rolling and cold rolling multipurpose rolling mills and tubular vacuum annealing furnaces. The specific operation of preparing the industrially pure titanium with the heterogeneous layered structure in this example is as follows:
(1) the thickness of the industrial pure titanium plate taken in the example is 15mm, and the components (wt.%) are as follows: 0.15O,0.01N,0.01C,0.03Fe, and the balance Ti and inevitable impurities.
(2) And (3) preserving the heat of the industrial pure titanium plate for 2 hours at 750 ℃ in a tubular vacuum annealing furnace to obtain a homogenized structure, wherein the average grain size of the homogenized structure is 70 microns.
(3) And (3) carrying out cold rolling treatment on the homogenized and annealed industrial pure titanium-titanium plate at room temperature, wherein the initial thickness is 15mm, the reduction per pass of rolling is 0.3-0.5 mm, the plate thickness is finally rolled to be 3mm, and the total rolling reduction is 80%.
(4) And (3) carrying out incomplete recrystallization annealing treatment on the industrial pure titanium plate subjected to cold rolling for 30min at 450 ℃ in a tubular vacuum annealing furnace.
(5) In this example, the yield strength of the industrially pure titanium with the heterogeneous layered structure obtained by the above method is 582MPa, the tensile strength is 630MPa, the uniform elongation is 6.4%, and the elongation at break is 21.2%. The engineering stress-engineering strain curves of the homogenized and annealed coarse-grain industrial pure titanium and the heterogeneous layered structure industrial pure titanium after cold rolling and incomplete recrystallization annealing are shown in fig. 3, and it can be seen that compared with the coarse-grain industrial pure titanium, the industrial pure titanium treated by the method of the present invention still has good plasticity and ductility, has good strength-plasticity matching, and can greatly promote industrial application.
Example two
First, the present embodiment adopts the following apparatus:
hot rolling and cold rolling multipurpose rolling mills and tubular vacuum annealing furnaces. The specific operation of preparing the industrially pure titanium with the heterogeneous layered structure in this example is as follows:
(1) the thickness of the industrial pure titanium plate taken in the example is 15mm, and the components (wt.%) are as follows: 0.15O,0.01N,0.01C,0.03Fe, and the balance Ti and inevitable impurities.
(2) And (3) preserving the heat of the industrial pure titanium plate for 2 hours at 750 ℃ in a tubular vacuum annealing furnace to obtain a homogenized structure, wherein the average grain size of the homogenized structure is 70 microns.
(3) And (3) carrying out cold rolling treatment on the homogenized and annealed industrial pure titanium-titanium plate at room temperature, wherein the initial thickness is 15mm, the reduction per pass of rolling is 0.3-0.5 mm, the plate thickness is finally rolled to be 3mm, and the total rolling reduction is 80%.
(4) And (3) carrying out incomplete recrystallization annealing treatment on the industrial pure titanium plate subjected to cold rolling for 60min at 450 ℃ in a tubular vacuum annealing furnace.
(5) In this example, the yield strength of the industrially pure titanium with the heterogeneous layered structure obtained by the above method was 590MPa, the tensile strength was 665MPa, the uniform elongation was 5.5%, and the elongation at break was 18.6%. The engineering stress-engineering strain curves of the homogenized and annealed coarse-grain industrial pure titanium and the heterogeneous layered structure industrial pure titanium after cold rolling and incomplete recrystallization annealing are shown in fig. 3, and it can be seen that compared with the coarse-grain industrial pure titanium, the industrial pure titanium treated by the method of the present invention still has good plasticity and ductility, has good strength-plasticity matching, and can greatly promote industrial application.
EXAMPLE III
First, the present embodiment adopts the following apparatus:
hot rolling and cold rolling multipurpose rolling mills and tubular vacuum annealing furnaces. The specific operation of preparing the industrially pure titanium with the heterogeneous layered structure in this example is as follows:
(1) the thickness of the industrial pure titanium plate taken in the example is 10mm, and the components (wt.%) are as follows: 0.15O,0.01N,0.01C,0.03Fe, and the balance Ti and inevitable impurities.
(2) And (3) preserving the heat of the industrial pure titanium plate for 2 hours at 750 ℃ in a tubular vacuum annealing furnace to obtain a homogenized structure, wherein the average grain size of the homogenized structure is 70 microns.
(3) And (3) carrying out cold rolling treatment on the homogenized and annealed industrial pure titanium-titanium plate at room temperature, wherein the initial thickness is 10mm, the reduction per pass of rolling is 0.3-0.5 mm, the plate thickness is finally rolled to be 1mm, and the total rolling reduction is 90%.
(4) And (3) carrying out incomplete recrystallization annealing treatment for 5min at 500 ℃ on the industrial pure titanium plate subjected to cold rolling in a tubular vacuum annealing furnace.
(5) In this example, the yield strength of the industrially pure titanium with the heterogeneous layered structure obtained by the above method is 660MPa, the tensile strength is 755MPa, the uniform elongation is 4.1%, and the elongation at break is 15.8%. The engineering stress-engineering strain curves of the homogenized and annealed coarse-grain industrial pure titanium and the heterogeneous layered structure industrial pure titanium after cold rolling and incomplete recrystallization annealing are shown in fig. 3, and it can be seen that compared with the coarse-grain industrial pure titanium, the industrial pure titanium treated by the method of the present invention still has good plasticity and ductility, has good strength-plasticity matching, and can greatly promote industrial application.
Claims (2)
1. A method for preparing industrial pure titanium with a heterogeneous layered structure is characterized by comprising the following steps:
(1) homogenizing annealing treatment
Annealing industrial pure titanium at 750 ℃ for 2h to obtain a homogenized structure, wherein the average grain size of the homogenized structure is about 70 mu m; the mass percentage of the industrial pure titanium is as follows: 0.15O,0.01N,0.01C,0.03Fe, and the balance of Ti and inevitable impurities;
(2) cold rolling treatment at room temperature
Polishing the homogenized and annealed industrial pure titanium-titanium plate by using sand paper, and then performing cold rolling treatment on the industrial pure titanium-titanium plate at room temperature, wherein the thickness of the original plate is 10-15 mm, the rolling reduction per pass is 0.3-0.5 mm, and the rolling reduction is 1-3 mm; the cold rolling treatment in the step (2) adopts a synchronous rolling mill, and the total cold rolling reduction at room temperature is 80-90%;
(3) annealing treatment for incomplete recrystallization
Annealing the cold-rolled industrial pure titanium at 450-500 ℃ for 5-60 min, and then air-cooling to room temperature; the annealing treatment adopts a tubular vacuum annealing furnace.
2. The industrially pure titanium with a heterogeneous layered structure prepared by the preparation method according to claim 1, wherein the industrially pure titanium is one in which a heterogeneous layered structure is formed by layering together ribbon-like aggregated recrystallized, refined ultrafine crystallites and elongated deformed coarse crystallites.
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| CN112522650A (en) * | 2020-12-09 | 2021-03-19 | 四川大学 | High-strength high-toughness superfine twin crystal pure titanium and preparation method thereof |
| CN115261670B (en) * | 2022-07-08 | 2023-07-07 | 四川大学 | High-strength and high-toughness pure titanium and preparation method thereof |
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|---|---|---|---|---|
| JP2001303223A (en) * | 2000-04-24 | 2001-10-31 | Sumitomo Metal Ind Ltd | Method for manufacturing titanium sheet excellent in formability |
| JP2011046995A (en) * | 2009-08-26 | 2011-03-10 | Nippon Steel Corp | Titanium alloy sheet having excellent press formability, method for producing the same, and titanium alloy sheet for heat exchanger |
| CN102909236A (en) * | 2012-11-14 | 2013-02-06 | 西部钛业有限责任公司 | Preparing method of wide-width pure titanium roll |
| CN106636747A (en) * | 2016-12-29 | 2017-05-10 | 广东技术师范学院 | Manufacturing method for producing commercial pure titanium plate by adopting double annealing of heavy and medium plate mill |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001303223A (en) * | 2000-04-24 | 2001-10-31 | Sumitomo Metal Ind Ltd | Method for manufacturing titanium sheet excellent in formability |
| JP2011046995A (en) * | 2009-08-26 | 2011-03-10 | Nippon Steel Corp | Titanium alloy sheet having excellent press formability, method for producing the same, and titanium alloy sheet for heat exchanger |
| CN102909236A (en) * | 2012-11-14 | 2013-02-06 | 西部钛业有限责任公司 | Preparing method of wide-width pure titanium roll |
| CN106636747A (en) * | 2016-12-29 | 2017-05-10 | 广东技术师范学院 | Manufacturing method for producing commercial pure titanium plate by adopting double annealing of heavy and medium plate mill |
Non-Patent Citations (1)
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| 冷轧工业纯钛的退火再结晶行为;徐国富 等;《稀有金属材料与工程》;20131130;第42卷(第11期);第2263页右栏，第2264页左栏 * |
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