CN113430409A - Preparation method of high-strength beta titanium alloy - Google Patents
Preparation method of high-strength beta titanium alloy Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-strength beta titanium alloy, which comprises the following steps: uniformly mixing Ti-15Mo alloy powder and Nb powder to obtain mixed powder; step (2), the mixed powder is filled into a plastic sheath and then is subjected to cold isostatic pressing treatment to obtain a metal pressed blank; step (3), carrying out high vacuum sintering treatment on the metal pressed compact to obtain a sintered titanium-molybdenum-niobium alloy; and (4) preheating the sintered titanium-molybdenum-niobium alloy, and immediately performing hot rolling to obtain the hot-rolled titanium-molybdenum-niobium alloy. The stability of the titanium alloy structure is improved by adding the beta stable element Nb, and the content of Nb and oxygen in the titanium alloy is controlled; by combining a sintering treatment process, a hot rolling treatment process and an annealing treatment process, the titanium alloy generates a large amount of stable beta phases and partial omega phases, so that the strength and the toughness of the titanium alloy are improved; finally obtaining the high-strength beta titanium alloy with low elastic modulus.
Description
Technical Field
The invention relates to a preparation method of a high-strength beta titanium alloy.
Background
In recent years, titanium alloy has high strength, good corrosion resistance and good biocompatibility, and is widely applied to the fields of aerospace and biomedical implants. Among various titanium alloys, the alpha type titanium alloy and the (alpha + beta) type titanium alloy have small density, higher strength and good thermal stability, so the alloy has common application in aerospace metal members, taking the (alpha + beta) type titanium alloy Ti-6Al-4V as an example, the yield strength of the alloy is about 850MPa at room temperature, the elongation is 7-10 percent, the elastic modulus reaches 110GPa, and the alloy is widely applied in the aerospace metal members and the biological field. However, the α type titanium alloy and the (α + β) type titanium alloy are inferior in cold forming and cold working. Compared with the prior art, the beta titanium alloy with thermal stability has more excellent cold processing performance, and the beta titanium alloy subjected to aging treatment generates a hard and brittle omega phase, so that the beta titanium alloy has higher strength and lower elastic modulus;
for beta titanium alloy, the addition of beta stabilizing elements such as Nb, Zr, Mo, Hf, Ta, etc. is beneficial to improving the strength of the alloy and reducing the elastic modulus of the alloy. Different kinds of beta stable elements have different influences on the performance of the titanium alloy, and researchers adopt diversified alloy design and combine with an optimized heat treatment process to improve the comprehensive performance of the titanium alloy. Alloy elements Nb and Zr are added into titanium base by casting by Shanghai university of transportation Jiaqing et al, the Zr content is changed, the elastic modulus of the alloy is reduced to 59-68 GPa, the elongation is increased, but the tensile strength and the yield strength are lower. Ti-29Nb-13Ta-4.6Zr developed in Japan leads alpha phase, omega phase and beta phase to appear in the alloy by increasing the content of more beta stabilizing elements, carrying out solid solution at 1073K temperature and carrying out subsequent aging treatment, the fatigue limit is about 700MPa, and the Young modulus is far lower than that of Ti-6Al-4V-ELI alloy;
in the design and development of the titanium alloy, the alloy is obtained by casting technology, the alloy is strengthened by solid solution and aging treatment, the yield strength of most of the obtained alloy is below 1GPa, even far below 1GPa, and the performances of plasticity, toughness and elastic modulus on the rest properties are not outstanding. Research on designing high-strength beta titanium alloy with good plasticity and low modulus by regulating and controlling sintering process, annealing process and heat treatment temperature is relatively lacked;
in addition, although the design and development of the titanium alloy have advantages, there are still many problems to be solved:
1. although the increase of the specific beta stabilizing element can improve the plasticity and reduce the elastic modulus of the material, the tensile strength and the yield strength of the alloy are also reduced;
2. the addition of more beta stable elements can cause the instability of the alloy structure, thereby influencing the structure in the processing process, changing the properties such as strength, plasticity and the like;
3. the medical titanium alloy can generate stress shielding effect due to the excessively high elastic modulus, and part of the titanium alloy containing the V element has certain toxicity to human bodies and can possibly cause other diseases.
Disclosure of Invention
The invention aims to provide a preparation method of a high-strength beta titanium alloy, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a high-strength beta titanium alloy comprises the following steps:
uniformly mixing Ti-15Mo alloy powder and Nb powder to obtain mixed powder;
step (2), the mixed powder is filled into a plastic sheath and then is subjected to cold isostatic pressing treatment to obtain a metal pressed blank;
step (3), carrying out high vacuum sintering treatment on the metal pressed compact to obtain a sintered titanium-molybdenum-niobium alloy;
step (4), preheating the sintered titanium-molybdenum-niobium alloy, and immediately performing hot rolling to obtain a hot-rolled titanium-molybdenum-niobium alloy;
and (5) annealing the hot-rolled titanium-molybdenum-niobium alloy in inert gas, and then performing water cooling treatment to obtain the high-strength beta titanium alloy.
In the step (1), the purity of the Ti-15Mo alloy powder is 99.7%, the purity of the Nb powder is 99.9%, the mass percentage of the Nb powder in the mixed powder is 0-13% of the total mass, and the mass percentage of Nb in the mixed powder is respectively selected from 0, 2.75%, 5.84% and 13%.
Further, in the step (2), the pressure of the cold isostatic pressing treatment is 100-400 MPa, the time of the cold isostatic pressing treatment is 1-5 min, the preferred pressure of the cold isostatic pressing treatment is 200-220 MPa, and the treatment time is 2-3 min, loose metal powder can be pressed into a pressed blank with certain strength under the preferred condition of the cold isostatic pressing treatment, the blank body is not pressed densely due to too low pressure or too short pressure maintaining time, the blank body is cracked, and the equipment cost is easily wasted due to too high pressure.
Further, in the step (3), the temperature of the high vacuum sintering treatment is 1200-1600 ℃, the heat preservation time of the high vacuum sintering treatment is 8-15 h, the optimal temperature of the high vacuum sintering treatment is 1400-1600 ℃, and the treatment heat preservation time is 10-12 h. 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.
Further, the preheating treatment in the step (4) is carried out at the temperature of 800-1000 ℃ for 10-60 min, the preferable temperature of the preheating treatment is 900-950 ℃ for 20-30 min, the preheating treatment before hot rolling can improve the plasticity of the alloy, reduce the deformation resistance and eliminate the original structural defects and stress, the phase transition temperature of the titanium molybdenum niobium alloy is 850-900 ℃, the temperature is increased to be higher than the temperature, and the preheating time is adjusted, so that the titanium molybdenum niobium alloy has enough time to homogenize the structure, and is convenient for subsequent rolling processing.
Further, in the step (4), the pass deformation of the hot rolling treatment is 1% -10% and the total rolling deformation is 1% -70%, the inter-pass recovery temperature of the hot rolling treatment is 850-900 ℃ and the inter-pass heat preservation time is 10-12 min, the pass deformation of the hot rolling treatment is preferably 5% -8% and the total rolling deformation is 60% -65%, the density of a sample can be greatly improved through the hot rolling treatment, and the influence of impurity oxygen elements on the performance of the material after processing can be reduced through high temperature. In addition, the alloy sample has large size change and is easy to crack due to excessively high pass deformation; the function of inter-pass heat preservation is mainly to eliminate the change of the environment to the temperature and keep the sample above the phase transition temperature.
Further, the protective gas in the step (5) is argon, and the preferable protective gas is argon in consideration of the possibility that nitrogen and titanium react to generate impurity compounds at high temperature.
Further, the annealing treatment temperature in the step (5) is 800-1100 ℃, the heat preservation time of the annealing treatment is 20-120 min, the preferred annealing treatment temperature is 900-1000 ℃, the heat preservation time of the annealing treatment is 40-80 min, and the annealing treatment is carried out above the phase transition temperature of the hot-rolled titanium alloy, so that alloy elements can be fully and uniformly diffused, and a stable single-phase beta phase can be obtained. Too short a holding time or too low a temperature to complete the transformation will result in instability of the beta phase of the alloy.
Further, in the step (5), the mass ratio of the components of alloy elements Ti and Mo in the high-strength beta titanium alloy is 85: 15, the content of an alloy element Nb in the high-strength beta titanium alloy accounts for 1-10% of the total mass of the high-strength beta titanium alloy.
Further, the high-strength beta titanium alloy in the step (5) contains 0.4-0.8 mass percent of oxygen element.
Compared with the prior art, the invention has the beneficial effects that: the stability of the titanium alloy structure is improved by adding a beta stabilizing element Nb, and the contents of Nb and oxygen in the titanium alloy are controlled; by combining a sintering treatment process, a hot rolling treatment process and an annealing treatment process, the titanium alloy generates a large amount of stable beta phases and partial omega phases, so that the strength and the toughness of the titanium alloy are improved; finally, the high-strength beta titanium alloy with low elastic modulus is obtained, and has the following obvious advantages:
1. the steps of the method of the invention, namely sintering, hot rolling and annealing treatment, are used for preparing the high-strength beta titanium alloy, so that the method is complete and easy to realize;
2. the element contained in the invention is beta stable element, Mo and Nb elements can form uniform solid solution with Ti element in a certain concentration range, and the single-phase alloy has more stable structure compared with two-phase alloy;
3. the invention is beta-type titanium alloy, which has excellent cold forming and cold processing performance;
4. the Mo and Nb elements contained in the invention have the advantages of no toxicity, no allergy and the like, have good biocompatibility with human bodies, and have excellent corrosion resistance.
Drawings
FIG. 1 is a mechanical property test chart of a high-strength beta titanium alloy in the second embodiment of the invention;
fig. 2 is a mechanical property test chart of the high-strength beta titanium alloy in the third embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a preparation method of a high-strength beta titanium alloy comprises the following steps:
step (1), Ti-15Mo alloy powder with the purity of 99.7% and Nb powder with the purity of 99.9% are used as raw materials, wherein the mass fraction of Nb is 0, and the raw materials do not contain other metal impurity elements;
step (2), filling Ti-15Mo alloy powder into a plastic sheath, and then carrying out cold isostatic pressing treatment to obtain a metal compact;
step (3), carrying out high vacuum sintering treatment on the metal pressed compact at 1200 ℃, and preserving heat for 4 hours to obtain a sintered Ti-15Mo alloy;
step (4), placing the sintered Ti-15Mo alloy in an electric heating furnace, preheating at 900 ℃, preserving heat for 30min, and immediately performing hot rolling to obtain the hot-rolled Ti-15Mo alloy, wherein the pass deformation of the hot rolling is about 7%, the total deformation is 65%, the hot rolling needs to be placed back to the electric heating furnace for temperature recovery between passes, the recovery temperature is 900 ℃, and the heat preservation time is controlled to be 10 min;
and (5) annealing the hot-rolled titanium Ti-15Mo alloy in an argon atmosphere at 900 ℃ for 60min, and then performing water cooling to obtain the annealed Ti-15Mo alloy, wherein the oxygen element content of the Ti-15Mo alloy is 0.2%.
The product of this example was tested by mechanical property testing, and the tensile strength of the annealed Ti-15Mo alloy after hot rolling in this example was: 810MPa, elongation 25% and elastic modulus 84 GPa.
Example two:
a preparation method of a high-strength beta titanium alloy comprises the following steps:
step (1), uniformly mixing Ti-15Mo alloy powder with the purity of 99.7% and Nb powder with the purity of 99.9% as raw materials, wherein the mass fraction of Nb is 2.75%, so as to obtain mixed powder, wherein the raw materials do not contain other metal impurity elements;
step (2), the mixed powder is filled into a plastic sheath and then is subjected to cold isostatic pressing treatment to obtain a metal pressed blank;
step (3), carrying out high vacuum sintering treatment on the metal pressed compact at 1400 ℃, and preserving heat for 12 hours to obtain a sintered Ti-14.6Mo-2.75Nb alloy;
step (4), placing the sintered Ti-14.6Mo-2.75Nb alloy in an electric heating furnace, carrying out preheating treatment at 900 ℃, preserving heat for 30min, and immediately carrying out hot rolling treatment to obtain the hot-rolled Ti-14.6Mo-2.75Nb alloy, wherein the pass deformation of the hot rolling treatment is about 7%, the total deformation is 65%, the pass needs to be placed back to the electric heating furnace for temperature recovery, the recovery temperature is 900 ℃, and the heat preservation time is controlled to be 10 min;
and (5) annealing the hot-rolled Ti-14.6Mo-2.75Nb alloy in an argon atmosphere at 900 ℃ for 60min, and then performing water cooling to obtain the annealed Ti-14.6Mo-2.75Nb alloy, namely the high-strength beta titanium alloy, wherein the oxygen element content of the Ti-14.6Mo-2.75Nb alloy is 0.42%.
The product of the present example was tested by room temperature tensile test, the mechanical properties of the annealed Ti-14.6Mo-2.75Nb alloy of the present example are shown in fig. 1, and the alloy was tested to have a tensile strength of 1148MPa, an elongation of 10.9%, and an elastic modulus of 72 GPa. Compared with Ti-15Mo alloy, the tensile strength of the material is greatly improved, the elongation is reduced, but the elastic modulus is reduced by 14%.
Example three:
a preparation method of a high-strength beta titanium alloy comprises the following steps:
step (1), uniformly mixing Ti-15Mo alloy powder with the purity of 99.7% and Nb powder with the purity of 99.9% as raw materials, wherein the mass fraction of Nb is 5.84%, so as to obtain mixed powder, wherein the raw materials do not contain other metal impurity elements;
step (2), the mixed powder is filled into a plastic sheath and then is subjected to cold isostatic pressing treatment to obtain a metal pressed blank;
step (3), carrying out high vacuum sintering treatment on the metal pressed compact at 1400 ℃, and preserving heat for 16 hours to obtain a sintered Ti-14.13Mo-5.84Nb alloy;
step (4), placing the sintered Ti-14.13Mo-5.84Nb alloy in an electric heating furnace, carrying out preheating treatment at 900 ℃, preserving heat for 30min, and immediately carrying out hot rolling treatment to obtain the hot-rolled Ti-14.13Mo-5.84Nb alloy, wherein the pass deformation of the hot rolling treatment is about 7%, the total deformation is 65%, the pass needs to be placed back to the electric heating furnace for temperature recovery, the recovery temperature is 900 ℃, and the heat preservation time is controlled to be 10 min;
and (5) annealing the hot-rolled Ti-14.13Mo-5.84Nb alloy in an argon atmosphere at 900 ℃ for 60min, and then performing water cooling to obtain the annealed Ti-14.13Mo-5.84Nb alloy, namely the high-strength beta titanium alloy, wherein the oxygen element content of the Ti-14.13Mo-5.84Nb alloy is not less than 0.45%.
The product of the embodiment is tested by a room temperature tensile test, the mechanical properties of the annealed Ti-14.13Mo-5.84Nb alloy of the embodiment are shown in a figure (2), and the alloy is detected to have the tensile strength of 1082MPa, the elongation of 8.63 percent and the elastic modulus of 72 GPa. Compared with Ti-15Mo alloy, the tensile strength of the material is improved to more than 1GPa, the tensile strength is improved by 33%, and the elastic modulus is reduced by 14%.
Example four:
a preparation method of a high-strength beta titanium alloy comprises the following steps:
step (1), uniformly mixing Ti-15Mo alloy powder with the purity of 99.7% and Nb powder with the purity of 99.9% as raw materials, wherein the mass fraction of the Nb powder is 13%, so as to obtain mixed powder, wherein the raw materials do not contain other metal impurity elements;
step (2), the mixed powder is filled into a plastic sheath and then is subjected to cold isostatic pressing treatment to obtain a metal pressed blank;
step (3), carrying out high vacuum sintering treatment on the metal pressed compact at 1400 ℃, and preserving heat for 10 hours to obtain a sintered Ti-13.05Mo-13Nb alloy;
step (4), placing the sintered alloy in an electric heating furnace, carrying out preheating treatment at 900 ℃, preserving heat for 30min, and immediately carrying out hot rolling treatment to obtain the hot-rolled Ti-13.05Mo-13Nb alloy, wherein the pass deformation of the hot rolling treatment is about 7%, the total deformation is 65%, the hot rolling treatment needs to be returned to the electric heating furnace for temperature recovery between passes, the recovery temperature is 900 ℃, and the heat preservation time is controlled to be 10 min;
and (5) annealing the hot-rolled Ti-13.05Mo-13Nb alloy in an argon atmosphere at 900 ℃ for 60min, and then performing water cooling to obtain the annealed Ti-13.05Mo-13Nb alloy, namely the high-strength beta titanium alloy, wherein the oxygen element content of the Ti-13.05Mo-13Nb alloy is 0.45%.
The product of this example was tested by room temperature tensile testing and the annealed Ti-13.05Mo-13Nb alloy of this example had a tensile strength of 900MPa, an elongation of 12% and an elastic modulus of 76 GPa. Compared with Ti-15Mo alloy, the tensile strength of the material is not obviously improved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A preparation method of high-strength beta titanium alloy is characterized by comprising the following steps: the method comprises the following steps:
uniformly mixing Ti-15Mo alloy powder and Nb powder to obtain mixed powder;
step (2), the mixed powder is filled into a plastic sheath and then is subjected to cold isostatic pressing treatment to obtain a metal pressed blank;
step (3), carrying out high vacuum sintering treatment on the metal pressed compact to obtain a sintered titanium-molybdenum-niobium alloy;
step (4), preheating the sintered titanium-molybdenum-niobium alloy, and immediately performing hot rolling to obtain a hot-rolled titanium-molybdenum-niobium alloy;
and (5) annealing the hot-rolled titanium-molybdenum-niobium alloy in inert gas, and then performing water cooling treatment to obtain the high-strength beta titanium alloy.
2. The method for preparing the high-strength beta titanium alloy according to claim 1, wherein the method comprises the following steps: in the step (1), the purity of the Ti-15Mo alloy powder is 99.7%, the purity of the Nb powder is 99.9%, and the mass fraction of the Nb powder in the mixed powder is within a range of 0-13%.
3. The method for preparing the high-strength beta titanium alloy according to claim 1, wherein the method comprises the following steps: the pressure of the cold isostatic pressing treatment in the step (2) is 100-400 MPa, and the time of the cold isostatic pressing treatment is 1-5 min.
4. The method for preparing the high-strength beta titanium alloy according to claim 1, wherein the method comprises the following steps: the temperature of the high vacuum sintering treatment in the step (3) is 1200-1600 ℃, and the heat preservation time of the high vacuum sintering treatment is 8-15 h.
5. The method for preparing the high-strength beta titanium alloy according to claim 1, wherein the method comprises the following steps: the temperature of the preheating treatment in the step (4) is 800-1000 ℃, and the treatment time is 10-60 min.
6. The method for preparing the high-strength beta titanium alloy according to claim 1, wherein the method comprises the following steps: in the step (4), the pass deformation of the hot rolling treatment is 1-10%, the total rolling deformation is 1-70%, the inter-pass recovery temperature of the hot rolling treatment is 850-900 ℃, and the inter-pass heat preservation time is 10-12 min.
7. The method for preparing the high-strength beta titanium alloy according to claim 1, wherein the method comprises the following steps: and (5) the inert gas is argon.
8. The method for preparing the high-strength beta titanium alloy according to claim 1, wherein the method comprises the following steps: the temperature of the annealing treatment in the step (5) is 800-1100 ℃, and the heat preservation time of the annealing treatment is 20-120 min.
9. The method for preparing the high-strength beta titanium alloy according to claim 1, wherein the method comprises the following steps: the mass ratio of the components of alloy elements Ti and Mo in the high-strength beta titanium alloy in the step (5) is 85: 15, the content of an alloy element Nb in the high-strength beta titanium alloy accounts for 1-10% of the total mass of the high-strength beta titanium alloy.
10. The method for preparing the high-strength beta titanium alloy according to claim 1, wherein the method comprises the following steps: in the step (5), the high-strength beta titanium alloy contains 0.4-0.8 mass percent of oxygen element.
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Cited By (3)
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|---|---|---|---|---|
| CN113909496A (en) * | 2021-09-28 | 2022-01-11 | 四川大学 | Preparation method of titanium alloy printed part of aircraft and thermal post-treatment of titanium alloy printed part |
| CN114888287A (en) * | 2022-04-08 | 2022-08-12 | 镇江力航新材料科技有限公司 | Pressed compact equipment for processing high-strength beta titanium alloy and using method thereof |
| CN115475946A (en) * | 2022-08-26 | 2022-12-16 | 贵州航宇科技发展股份有限公司 | Ti 2 Roll forming and heat treatment method of AlNb powder metallurgy ring piece |
-
2021
- 2021-07-19 CN CN202110814579.5A patent/CN113430409A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113909496A (en) * | 2021-09-28 | 2022-01-11 | 四川大学 | Preparation method of titanium alloy printed part of aircraft and thermal post-treatment of titanium alloy printed part |
| CN114888287A (en) * | 2022-04-08 | 2022-08-12 | 镇江力航新材料科技有限公司 | Pressed compact equipment for processing high-strength beta titanium alloy and using method thereof |
| CN114888287B (en) * | 2022-04-08 | 2024-01-23 | 镇江力航新材料科技有限公司 | Compacting equipment for processing high-strength beta titanium alloy and using method thereof |
| CN115475946A (en) * | 2022-08-26 | 2022-12-16 | 贵州航宇科技发展股份有限公司 | Ti 2 Roll forming and heat treatment method of AlNb powder metallurgy ring piece |
| CN115475946B (en) * | 2022-08-26 | 2024-04-02 | 贵州航宇科技发展股份有限公司 | Ti (titanium) 2 Rolling forming and heat treatment method for AlNb powder metallurgy ring piece |
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