CN111004987B - Method for regulating and controlling mechanical property of metastable beta titanium alloy - Google Patents
Method for regulating and controlling mechanical property of metastable beta titanium alloy Download PDFInfo
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- CN111004987B CN111004987B CN201911375416.0A CN201911375416A CN111004987B CN 111004987 B CN111004987 B CN 111004987B CN 201911375416 A CN201911375416 A CN 201911375416A CN 111004987 B CN111004987 B CN 111004987B
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Abstract
The invention discloses a method for regulating and controlling mechanical properties of metastable beta titanium alloy, which comprises the steps of cutting a metastable beta titanium alloy material into plates, and removing a surface oxide layer to obtain the metastable beta titanium alloy plates; carrying out cryogenic treatment on the metastable beta titanium alloy plate; carrying out pre-deformation processing on the metastable beta titanium alloy plate subjected to the cryogenic treatment; and (3) putting the pre-deformed and processed metastable beta titanium alloy in air to restore to room temperature, thus obtaining the metastable titanium alloy containing the twin structure. The method jointly realizes the regulation and control of the microstructure of the metastable titanium alloy through the temperature effect in the cryogenic treatment and the stress action in the processing process, and induces a large amount of twin tissues in the alloy. The twin structure has obvious effect of improving the strength and plasticity of the alloy and realizes the strengthening and toughening of the metastable beta titanium alloy.
Description
Technical Field
The invention relates to a method for regulating and controlling mechanical properties of a metastable beta titanium alloy, in particular to a method for regulating and controlling strength and plasticity of the metastable beta titanium alloy by using a technology combining cryogenic treatment and pre-deformation processing, belonging to the technical field of metal material processing.
Background
The metastable beta titanium alloy has good heat treatment response, welding performance, excellent mechanical property and processing performance, and is increasingly applied to the high-tech fields of aerospace aircrafts and the like and the national economy fields of energy sources, ships, automobiles and the like. In addition, the metastable beta titanium alloy also has lower elastic modulus, excellent corrosion resistance, good biocompatibility, shape memory effect and the like, and is considered to be a biomedical material with wide application prospect. For metastable beta titanium alloy with body-centered cubic structure, large deformation is the most common method for realizing the optimization of mechanical properties. For example: the Ti-36Nb-2Ta-3Zr-0.35O alloy (TNTZO, also called as rubber alloy) is subjected to cold rotary swaging processing with the area percentage of 90%, the tensile strength of the alloy is improved from about 900MPa to 1100MPa, the elastic modulus is reduced to 55GPa, the alloy has nonlinearity and superelasticity of about 2.5%, and the excellent performances of Invar, Elinvar and the like are shown. The Shenyang metal Yankee et al, after a large thermal deformation (machining of the rod diameter from 280mm to 12mm) allows the metastable beta titanium alloy Ti2448 to obtain its series of excellent mechanical properties.
In addition, researchers also adopt methods such as heat treatment, equal channel angular extrusion and the like to toughen the metastable beta titanium alloy. The metastable Ti-10V-2Fe-3Al alloy is subjected to heat treatment in a beta phase region or an alpha + beta dual-phase region by Zhao Xinqing and the like at Beijing aerospace university, so that a hard and brittle omega phase is formed in the alloy, the strength of the alloy is greatly improved, and the elongation is obviously reduced. Shanghai university of transportation, Lvvirejie et al, induced martensite transformation of Ti-35Nb-2Ta-3Zr alloy by ECAP processing, further increased tensile strength (534MPa to 765MPa), while the alloy still maintained 16% elongation.
The method for regulating and controlling the mechanical property of the metastable beta titanium alloy mostly focuses on regulating and controlling the alloy property through heat action (heat treatment), force action (deformation processing) and combination of the heat action and the force action (deformation processing), and research on realizing the regulation and control of the mechanical property of the metastable beta titanium alloy through a method combining cryogenic treatment and deformation processing is lacked.
In addition, although the methods for regulating the mechanical properties of the metastable beta titanium alloy have various advantages, more problems still remain to be solved:
1. after large deformation, the metastable beta titanium alloy test piece has smaller size (taking TNTZO as an example: the diameter of the alloy bar after large deformation is about 5mm), and the application of the metastable beta titanium alloy test piece in the fields of automobiles, medical instruments, sports products and the like is greatly limited.
2. The heat treatment method can singly improve the strength or plasticity of the metastable beta titanium alloy, but cannot meet the requirements of both high strength and high toughness.
3. Due to the size limitations of ECAP dies, the shape and size of the metal blanks obtained are also very limited.
Disclosure of Invention
The invention aims to provide a method for processing metastable beta titanium alloy by using a combined process of cryogenic treatment and pre-deformation, which realizes the regulation of mechanical property of the metastable beta titanium alloy through temperature effect and stress coupling, and realizes the strengthening and toughening of a large amount of twin tissues induced in the metastable beta titanium alloy by inducing a large amount of twin tissues, aiming at the problems that in the prior art, a metastable beta titanium alloy test piece obtained after the metastable beta titanium alloy is subjected to large deformation has a small size (taking TNTZO as an example, the diameter of an alloy bar after the large deformation is about 5mm), the application is limited, the heat treatment cannot meet the requirement of both high strength and high toughness, the shape and the size of a metal blank obtained after ECAP processing are limited, and the like.
In order to achieve the technical purpose, the invention provides a method for regulating and controlling the mechanical property of a metastable beta titanium alloy, which comprises the following steps:
1) cutting the metastable beta titanium alloy material into plates, and removing a surface oxidation layer to obtain the metastable beta titanium alloy plate;
2) carrying out cryogenic treatment on the metastable beta titanium alloy plate;
3) carrying out pre-deformation processing on the metastable beta titanium alloy plate subjected to the cryogenic treatment;
4) and (3) putting the pre-deformed and processed metastable beta titanium alloy in air to restore to room temperature, thus obtaining the metastable titanium alloy containing the twin structure.
In a preferable scheme, the equivalent weight of the alloy element molybdenum in the metastable beta titanium alloy is within a range of 10-25.
Preferably, the metastable beta titanium alloy contains a trace impurity oxygen element with the mass percentage of less than 0.4 percent.
In a preferred scheme, the condition of the cryogenic treatment is as follows: the temperature is 77K to 273K, and the time is 1min to 60 min. In a more preferable scheme, the condition of the cryogenic treatment is as follows: the temperature is 77K-200K, and the time is 15 min-40 min. Under the condition of optimal cryogenic treatment, the beta phase stability in the metastable beta titanium alloy can be further reduced without modifying the integration of gold components, and the possibility of phase transformation and twinning tissue induction in the alloy is increased. Too high cryogenic treatment temperature increases the stability of the beta phase in the alloy, and thus cannot induce strengthening and toughening of the structure. Too short a holding time is not sufficient to make the internal temperature of the alloy uniform, which may result in inconsistent beta-phase stability in the alloy.
Preferably, the conditions of the pre-deformation processing are as follows: the pass deformation is 1-5%, the total rolling deformation is 1-35%, and the inter-pass recovery temperature is 77-273K. More preferably, the conditions of the pre-deformation processing are as follows: the pass deformation is 3-5%, the total rolling deformation is 3-15%, and the inter-pass recovery temperature is 77-200K. Under the preferable deformation processing conditions, the change range of the external dimension of the processed sample is small, and the alloy sample with larger dimension can be obtained. In addition, the stress effects during machining can induce twinning in the alloy which can enhance toughening. The effect of the inter-pass recovery temperature is mainly to eliminate the thermal effect caused by processing and keep the sample in the low temperature state of the cryogenic treatment. Too high rolling deformation will result in large changes in the alloy dimensions, limiting its application.
In the preferable scheme, the inter-pass recovery temperature in the pre-deformation processing process is not higher than the temperature in the cryogenic treatment process.
The key point of the technical scheme of the invention is that the beta phase stability of the metastable beta titanium alloy is further reduced by using cryogenic treatment, and the possibility of phase change or twin crystal induction in the alloy is increased; then inducing a large amount of twin tissues in the alloy by applying the stress action applied by the pre-deformation processing; then the purposes of grain refinement and twin plasticization are achieved through a twin structure, and finally the metastable beta titanium alloy with excellent comprehensive performance of strength and elongation is obtained. Compared with the similar process in the prior art, the method has the following obvious advantages:
(1) the process steps comprise cryogenic treatment and stress action regulation and control of the mechanical property of the metastable beta titanium alloy, and are complete and easy to realize.
(2) The change of the shape and the size of the metastable beta titanium alloy can be effectively controlled, and an alloy sample with larger size can be obtained.
(3) The density of twin structures in the metastable beta titanium alloy can be effectively controlled through the cryogenic treatment temperature and the processing deformation, and the aim of regulating and controlling the mechanical property of the metastable beta titanium alloy is further fulfilled.
(4) The twin structure greatly contributes to the improvement of the alloy strength and the plasticity, and the good matching of the metastable beta titanium alloy strength and the plasticity can be realized.
Drawings
FIG. 1 shows the morphology and mechanical properties of the raw materials used in example 1 of the present invention.
FIG. 2 is a metastable beta titanium alloy structure after low temperature pre-deformation (3.2%) in example 1 of the present invention.
FIG. 3 is the mechanical properties of the metastable beta titanium alloy after low temperature pre-deformation (3.2%) in example 1 of the present invention.
FIG. 4 is a metastable beta titanium alloy structure after room temperature pre-deformation (4.5%) in example 5 of the present invention.
FIG. 5 is the mechanical properties of the metastable beta titanium alloy after room temperature pre-deformation (4.5%) in example 5 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
The method for regulating and controlling the mechanical property of the metastable beta titanium alloy comprises the following steps:
(1) ti-36Nb-2Ta-3Zr-0.35O bar is used as a raw material, and the [ Mo ] equivalent is 11.41. The alloy is free of other metal impurity elements except a small amount of inevitable impurity oxygen elements; cutting the Ti-36Nb-2Ta-3Zr-0.35O bar into plates suitable for rolling by using wire cut electrical discharge machining, and removing a surface oxidation layer. The dimensions are approximately 60mm by 10mm by 2 mm.
(2) And (2) placing the Ti-36Nb-2Ta-3Zr-0.35O alloy plate with a clean surface in the step (1) into a cryogenic insulation box, and carrying out cryogenic treatment, wherein the temperature in the cryogenic insulation box is maintained by liquid nitrogen. The subzero treatment process is characterized in that the temperature is controlled to be 77K, and the heat preservation time is controlled to be 30 min;
(3) and (3) taking the prepared Ti-36Nb-2Ta-3Zr-0.35O alloy plate subjected to the deep cooling treatment in the step (2) out of the deep cooling heat preservation box, immediately performing rolling pre-deformation, wherein the pass deformation is about 1%, the total deformation is 3.5%, the temperature needs to be restored by putting the plate back to the deep cooling heat preservation box in the pass, the restoration temperature is 200K, and the time is controlled to be 5 min. After pre-deformation, placing the alloy plate in the air, and recovering the alloy plate to room temperature to obtain a pre-deformed Ti-36Nb-2Ta-3Zr-0.35O alloy plate;
the product of this example is tested by a structure observation method, the structure after deep cooling treatment and pre-deformation of the metastable beta titanium alloy of this example is shown in fig. 3, and it can be known that compared with the structure before treatment (fig. 1), the metastable beta titanium alloy of this example is effectively regulated and controlled, and the alloy plate contains a large amount of twin structures. As can be seen from FIG. 4, the metastable beta titanium alloy regulated and controlled by the invention has good performance, and the tensile strength of the material is detected as follows: 907MPa and elongation rate of 16.5 percent. The strength of the alloy plate is 10 percent higher than that of the alloy plate before treatment (the tensile strength is 825MPa, and the elongation is 10 percent), and the elongation is 65 percent higher.
Example 2
The method for regulating and controlling the mechanical property of the metastable beta titanium alloy comprises the following steps:
(1) ti-36Nb-2Ta-3Zr-0.35O bar is used as a raw material, and the [ Mo ] equivalent is 11.41. The alloy is free of other metal impurity elements except a small amount of inevitable impurity oxygen elements; cutting the Ti-36Nb-2Ta-3Zr-0.35O bar into plates suitable for rolling by using wire cut electrical discharge machining, and removing a surface oxidation layer. The dimensions are approximately 60mm by 10mm by 2 mm.
(2) And (2) placing the Ti-36Nb-2Ta-3Zr-0.35O alloy plate with a clean surface in the step (1) into a cryogenic insulation box, and carrying out cryogenic treatment, wherein the temperature in the cryogenic insulation box is maintained by liquid nitrogen. The subzero treatment process is characterized in that the temperature is controlled to be 77K, and the heat preservation time is controlled to be 30 min;
(3) and (3) taking the prepared Ti-36Nb-2Ta-3Zr-0.35O alloy plate subjected to the deep cooling treatment in the step (2) out of the deep cooling heat preservation box, immediately performing rolling pre-deformation, wherein the pass deformation is about 2%, the total deformation is 6.5%, the temperature needs to be restored by putting the plate back to the deep cooling heat preservation box in the pass, the restoration temperature is 200K, and the time is controlled to be 5 min. After pre-deformation, placing the alloy plate in the air, and recovering the alloy plate to room temperature to obtain a pre-deformed Ti-36Nb-2Ta-3Zr-0.35O alloy plate;
the product of the embodiment is tested by a structure observation method, and the metastable beta titanium alloy plate containing a large amount of twin structures is finally obtained by the regulating and controlling process. Through detection, the tensile strength of the material is as follows: 910MPa, and the elongation is 18 percent.
Example 3
The method for regulating and controlling the mechanical property of the metastable beta titanium alloy comprises the following steps:
(1) ti-36Nb-2Ta-3Zr-0.35O bar is used as a raw material, and the [ Mo ] equivalent is 11.41. The alloy is free of other metal impurity elements except a small amount of inevitable impurity oxygen elements; cutting the Ti-36Nb-2Ta-3Zr-0.35O bar into plates suitable for rolling by using wire cut electrical discharge machining, and removing a surface oxidation layer. The dimensions are approximately 60mm by 10mm by 2 mm.
(2) And (2) placing the Ti-36Nb-2Ta-3Zr-0.35O alloy plate with a clean surface in the step (1) into a cryogenic insulation box, and carrying out cryogenic treatment, wherein the temperature in the cryogenic insulation box is maintained by liquid nitrogen. The subzero treatment process is characterized in that the temperature is controlled to be 77K, and the heat preservation time is controlled to be 30 min;
(3) and (3) taking the prepared Ti-36Nb-2Ta-3Zr-0.35O alloy plate subjected to the deep cooling treatment in the step (2) out of the deep cooling heat preservation box, immediately performing rolling pre-deformation, wherein the pass deformation is about 3%, the total deformation is 9%, the plate needs to be placed back into the deep cooling heat preservation box for temperature recovery in the pass, the recovery temperature is 77K, and the time is controlled to be 5 min. After pre-deformation, placing the alloy plate in the air, and recovering the alloy plate to room temperature to obtain a pre-deformed Ti-36Nb-2Ta-3Zr-0.35O alloy plate;
the product of the embodiment is tested by a structure observation method, and the metastable beta titanium alloy plate containing a large amount of twin structures is finally obtained by the regulating and controlling process. Through detection, the tensile strength of the material is as follows: 920MPa and an elongation of 15 percent.
Example 4
The method for regulating and controlling the mechanical property of the metastable beta titanium alloy comprises the following steps:
(1) ti-36Nb-2Ta-3Zr-0.35O bar is used as a raw material, and the [ Mo ] equivalent is 11.41. The alloy is free of other metal impurity elements except a small amount of inevitable impurity oxygen elements; cutting the Ti-36Nb-2Ta-3Zr-0.35O bar into plates suitable for rolling by using wire cut electrical discharge machining, and removing a surface oxidation layer. The dimensions are approximately 60mm by 10mm by 2 mm.
(2) And (2) placing the Ti-36Nb-2Ta-3Zr-0.35O alloy plate with a clean surface in the step (1) into a cryogenic insulation box, and carrying out cryogenic treatment, wherein the temperature in the cryogenic insulation box is maintained by liquid nitrogen. The subzero treatment process is to control the temperature to be 200K and the heat preservation time to be 40 min;
(3) and (3) taking the prepared Ti-36Nb-2Ta-3Zr-0.35O alloy plate subjected to the deep cooling treatment in the step (2) out of the deep cooling heat preservation box, immediately performing rolling pre-deformation, wherein the pass deformation is about 3%, the total deformation is 6%, the plate needs to be placed back into the deep cooling heat preservation box for temperature recovery in the pass, the recovery temperature is 200K, and the time is controlled to be 10 min. After pre-deformation, placing the alloy plate in the air, and recovering the alloy plate to room temperature to obtain a pre-deformed Ti-36Nb-2Ta-3Zr-0.35O alloy plate;
the product of the embodiment is tested by a structure observation method, and the metastable beta titanium alloy plate containing a large amount of twin structures is finally obtained by the regulating and controlling process. Through detection, the tensile strength of the material is as follows: 905MPa and elongation of 15.2%.
Example 5
The method for regulating and controlling the mechanical property of the metastable beta titanium alloy comprises the following steps:
(1) ti-36Nb-2Ta-3Zr-0.35O bar is used as raw material, and the equivalent weight of Mo is. In addition, the alloy does not contain other metal impurity elements except a small amount of inevitable impurity oxygen elements; cutting the Ti-36Nb-2Ta-3Zr-0.35O bar into plates suitable for rolling by using wire cut electrical discharge machining, and removing a surface oxidation layer. The dimensions are approximately 60mm by 10mm by 2 mm.
(2) And (2) placing the Ti-36Nb-2Ta-3Zr-0.35O alloy plate with clean surface in the step (1) into a cryogenic insulation box, and maintaining the temperature in the cryogenic insulation box by pure water. The treatment process is that the temperature is controlled to be 298K, and the heat preservation time is controlled to be 30 min;
(3) and (3) taking the prepared Ti-36Nb-2Ta-3Zr-0.35O alloy plate subjected to the deep cooling treatment in the step (2) out of the deep cooling heat preservation box, immediately performing rolling pre-deformation, wherein the pass deformation is about 1.5%, the total deformation is 4.5%, the temperature needs to be restored to 298K in the pass through the deep cooling heat preservation box, and the time is controlled to 10 min. Finally obtaining a pre-deformed Ti-36Nb-2Ta-3Zr-0.35O alloy plate;
the product of this example was tested by a structure observation method, and the structure of the metastable beta titanium alloy after deep cooling and pre-deformation in this example is shown in fig. 5, and it can be known from the above photographs that the structure of the metastable beta titanium alloy before and after pre-deformation in this example does not change significantly and a large amount of twinning structures do not appear. As can be seen from FIG. 6, the regulated metastable beta titanium alloy of the invention has worse performance than the above examples, and the tensile strength of the material is detected as follows: 870MPa and an elongation of 14.5 percent.
Example 6
The method for regulating and controlling the mechanical property of the metastable beta titanium alloy comprises the following steps:
(1) ti-36Nb-2Ta-3Zr-0.35O bar is used as raw material, and the equivalent weight of Mo is. In addition, the alloy does not contain other metal impurity elements except a small amount of inevitable impurity oxygen elements; cutting the Ti-36Nb-2Ta-3Zr-0.35O bar into plates suitable for rolling by using wire cut electrical discharge machining, and removing a surface oxidation layer. The dimensions are approximately 60mm by 10mm by 2 mm.
(2) And (2) placing the Ti-36Nb-2Ta-3Zr-0.35O alloy plate with clean surface in the step (1) into a cryogenic insulation box, and maintaining the temperature in the cryogenic insulation box by pure water. The treatment process comprises controlling the temperature at 77K and the heat preservation time at 30 min;
(3) and (3) taking the prepared Ti-36Nb-2Ta-3Zr-0.35O alloy plate subjected to the deep cooling treatment in the step (2) out of the deep cooling heat preservation box, immediately performing rolling pre-deformation, wherein the pass deformation is about 5%, the total deformation is 40%, the plate needs to be placed back into the deep cooling heat preservation box for temperature recovery in the pass, the recovery temperature is 77K, and the time is controlled to be 5 min. Finally obtaining a pre-deformed Ti-36Nb-2Ta-3Zr-0.35O alloy plate;
in the embodiment, the metastable beta titanium alloy grains are seriously flattened and elongated before and after pre-deformation, a large amount of slip band tissues appear, but a large amount of twin tissues do not appear. The test shows that the tensile strength of the material is slightly improved, but the elongation is greatly reduced (the tensile strength of the material is 1000MPa, and the elongation is 3.7%).
Claims (1)
1. A method for regulating and controlling the mechanical property of metastable beta titanium alloy is characterized in that: the method comprises the following steps:
1) cutting the metastable beta titanium alloy material into plates, and removing a surface oxidation layer to obtain the metastable beta titanium alloy plate; the equivalent weight of the alloy element molybdenum in the metastable beta titanium alloy is within the range of 10-25; the metastable beta titanium alloy contains trace impurity oxygen with the mass percentage lower than 0.4 percent;
2) carrying out cryogenic treatment on the metastable beta titanium alloy plate; the condition of the cryogenic treatment is as follows: the temperature is 77K-200K, and the time is 15 min-40 min;
3) carrying out pre-deformation processing on the metastable beta titanium alloy plate subjected to the cryogenic treatment; the conditions of the pre-deformation processing are as follows: the pass deformation is 3% -5%, the rolling total deformation is 3% -15%, and the inter-pass recovery temperature is 77K-200K; the inter-pass recovery temperature in the pre-deformation processing process is not higher than the temperature in the cryogenic treatment process;
4) and (3) putting the pre-deformed and processed metastable beta titanium alloy in air to restore to room temperature, thus obtaining the metastable titanium alloy containing the twin structure.
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