A multi-component titanium alloy, its preparation method and application

Abstract

This invention discloses a multi-component titanium alloy, its preparation method, and its applications, comprising the following components by mass percentage: tungsten 15-30%; zirconium 3-15%; molybdenum 2-10%; with the balance being titanium and unavoidable impurities. The multi-component titanium alloy provided by this invention exhibits high plasticity, high strength, and good X-ray visibility. This multi-component titanium alloy, composed of non-biotoxic elements Ti, W, Mo, and Zr, possesses excellent biocompatibility.

Description

Technical Field

[0001] This invention relates to the field of alloy materials technology, and in particular to a multi-component titanium alloy, its preparation method, and its applications. Background Technology

[0002] Titanium alloys have high biocompatibility, making them an ideal material for human implantation. However, traditional titanium alloys cannot simultaneously achieve high strength and high ductility, and their visibility under X-rays is low, thus limiting their application in cardiovascular stents. Therefore, it is necessary to design and fabricate novel titanium alloys that combine high strength, high ductility, and excellent visibility. Summary of the Invention

[0003] The present invention aims to at least solve one of the technical problems existing in the prior art. To this end, the first aspect of the present invention proposes a multi-component titanium alloy, which has high X-ray impermeability, high strength and ductility, and high strength.

[0004] A second aspect of the present invention also provides a method for preparing a multi-component titanium alloy.

[0005] A third aspect of the present invention also provides an application of a multi-element titanium alloy.

[0006] According to a first aspect of the present invention, a multi-component titanium alloy comprises the following components calculated by mass percentage:

[0007] Tungsten (W) 15-30%; Zirconium (Zr) 3-15%; Molybdenum (Mo) 2-10%; balance is titanium (Ti) and unavoidable impurities.

[0008] The multi-component titanium alloy according to embodiments of the present invention has at least the following beneficial effects:

[0009] The multi-component titanium alloy provided by this invention exhibits high plasticity, high strength, and X-ray visibility. This is because by altering the proportions of Ti, W, Zr, and Mo, the multi-component titanium alloy achieves a single-phase metastable β-phase matrix after quenching. During deformation, the metastable β-phase matrix undergoes a β→α" martensitic transformation and / or mechanical twinning, where α" is an orthorhombic martensitic phase. The β→α" martensitic transformation and mechanical twinning introduce transformation-induced plasticity, twinning-induced plasticity, transformation-induced work hardening, and twinning-induced plasticity into the multi-component titanium alloy, resulting in a plasticity exceeding 25%.

[0010] Furthermore, the present invention introduces tungsten and limits the mass percentage of tungsten, which can significantly improve the X-ray impermeability of multi-component titanium alloys.

[0011] Furthermore, the multi-component titanium alloy of the present invention is composed of non-biotoxic elements Ti, W, Mo and Zr, and has excellent biocompatibility.

[0012] According to some embodiments of the present invention, the components include the following components calculated by mass percentage:

[0013] Tungsten 18-24%; Zirconium 3-7%; Molybdenum 3-5%; Balance titanium and unavoidable impurities.

[0014] The method for preparing a multi-component titanium alloy according to a second aspect embodiment of the present invention includes the following steps:

[0015] S1. Weigh tungsten, zirconium, molybdenum and titanium and melt them into alloy ingots;

[0016] S2. The alloy ingot from step S1 is cold-rolled and deformed into a slab.

[0017] S3. The plate is solution treated and then quenched and cooled to room temperature.

[0018] According to some embodiments of the present invention, in step S3, the solution temperature of the solution treatment is 900℃~1200℃.

[0019] According to some embodiments of the present invention, in step S3, the heat preservation time of the solution treatment is 5 min to 60 min.

[0020] According to some embodiments of the present invention, in step S3, the solution treatment is performed in a vacuum environment.

[0021] According to some embodiments of the present invention, in step S2, the deformation amount of the cold rolling deformation is greater than 90%.

[0022] According to some embodiments of the present invention, in step S3, the cooling rate is 550°C / s to 650°C / s.

[0023] According to some embodiments of the present invention, in step S1, the melting temperature is 3000℃~3200℃.

[0024] According to some embodiments of the present invention, in step S1, the smelting is performed several times.

[0025] According to some embodiments of the present invention, in step S1, the smelting apparatus is a non-consumable vacuum electric arc furnace.

[0026] According to some embodiments of the present invention, in step S3, the apparatus used for the solution treatment is a heat treatment furnace or a vacuum quenching furnace.

[0027] According to some embodiments of the present invention, the purity of the zirconium, titanium, tungsten, and molybdenum elements is ≥99.9 wt%.

[0028] A third aspect of this invention provides the application of the aforementioned multi-principal alloy in the preparation of biomedical materials.

[0029] Other features and advantages of the invention will be set forth in the description which follows, and will be apparent in part from the description, or may be learned by practicing the invention. Attached Figure Description

[0030] The above and / or additional aspects and advantages of the present invention will become apparent and readily understood from the description of the embodiments taken in conjunction with the following drawings, in which:

[0031] Figure 1 This is a SEM image of Embodiment 1 (Ti-18W-8Zr-3Mo) of the present invention;

[0032] Figure 2 This is a SEM image of Embodiment 1 (Ti-18W-8Zr-3Mo) of the present invention after tensile deformation; Detailed Implementation

[0033] The following are specific embodiments of the present invention, and the technical solutions of the present invention will be further described in conjunction with the embodiments, but the present invention is not limited to these embodiments.

[0034] Unless otherwise specified, the reagents, methods and equipment used in this invention are all conventional reagents, methods and equipment in this technical field.

[0035] Industrial pure metals with a purity of 99.9% or higher by mass are selected as raw materials.

[0036] Example 1

[0037] Example 1 provides a multi-element titanium alloy, the mass percentage of each element of which is shown in Table 1, and its preparation method is as follows:

[0038] S1. Weigh zirconium, tungsten, molybdenum and titanium according to the element mass percentage and place them in a magnetic stirring vacuum non-consumable arc furnace for repeated melting five times (3200℃, 1min each time), and vacuum cast them into ingots with uniform composition.

[0039] S2. The alloy ingot from step S1 is cold-rolled and deformed into a plate with a thickness of 1.5 mm and a deformation amount of 95%.

[0040] S3. The plate is solution treated (950℃ for 1h), and then quenched and cooled to room temperature to obtain a multi-principal element alloy (named: Ti-18W-8Zr-3Mo).

[0041] The multi-component titanium alloy of Example 1 of the present invention was subjected to SEM testing, and the results are as follows: Figure 1The obtained multi-component titanium alloy was subjected to tensile testing, followed by SEM analysis. The results are shown in the figure. Figure 2 ,from Figure 1 As can be seen, the above heat treatment can yield a single-phase BCC. Figure 2 As can be seen, α" martensite and twins can be obtained during the tensile deformation process, thus achieving excellent mechanical properties.

[0042] Example 2

[0043] Example 2 provides a multi-element titanium alloy, the mass percentage of each element of which is shown in Table 1, and its preparation method is as follows:

[0044] S1. Weigh zirconium, tungsten, molybdenum and titanium according to the element mass percentage and place them in a magnetic stirring vacuum non-consumable arc furnace for repeated melting five times (3200℃, 1min each time), and vacuum cast them into ingots with uniform composition.

[0045] S2. The alloy ingot from step S1 is cold-rolled and deformed into a plate with a thickness of 1.5 mm and a deformation amount of 95%.

[0046] S3. The plate is solution treated (950℃ for 1h), and then quenched and cooled to room temperature to obtain a multi-principal element alloy (named: Ti-22W-4Zr-3Mo).

[0047] Example 3

[0048] Example 3 provides a multi-element titanium alloy, the mass percentage of each element of which is shown in Table 1, and its preparation method is as follows:

[0049] S1. Weigh zirconium, tungsten, molybdenum and titanium according to the element mass percentage and place them in a magnetic stirring vacuum non-consumable arc furnace for repeated melting five times (3200℃, 1min each time), and vacuum cast them into ingots with uniform composition.

[0050] S2. The alloy ingot from step S1 is cold-rolled and deformed into a plate with a thickness of 1.5 mm and a deformation amount of 95%.

[0051] S3. The plate is solution treated (950℃ for 1h), and then quenched and cooled to room temperature to obtain a multi-principal element alloy (named: Ti-25W-4Zr-5Mo).

[0052] Example 4

[0053] Example 4 provides a multi-element titanium alloy, the mass percentage of each element of which is shown in Table 1, and its preparation method is as follows:

[0054] S1. Weigh zirconium, tungsten, molybdenum and titanium according to the element mass percentage and place them in a magnetic stirring vacuum non-consumable arc furnace for repeated melting five times (3200℃, 1min each time), and vacuum cast them into ingots with uniform composition.

[0055] S2. The alloy ingot from step S1 is cold-rolled and deformed into a plate with a thickness of 1.5 mm and a deformation amount of 95%.

[0056] S3. The plate is solution treated (950℃ for 1h), and then quenched and cooled to room temperature to obtain a multi-principal element alloy (named: Ti-22W-5Zr-3Mo).

[0057] Example 5

[0058] Example 5 provides a multi-element titanium alloy, the mass percentage of each element of which is shown in Table 1, and its preparation method is as follows:

[0059] S1. Weigh zirconium, tungsten, molybdenum and titanium according to the element mass percentage and place them in a magnetic stirring vacuum non-consumable arc furnace for repeated melting five times (3200℃, 1min each time), and vacuum cast them into ingots with uniform composition.

[0060] S2. The alloy ingot from step S1 is cold-rolled and deformed into a plate with a thickness of 1.5 mm and a deformation amount of 95%.

[0061] S3. The plate is solution treated (950℃ for 1h), and then quenched and cooled to room temperature to obtain a multi-principal element alloy (named: Ti-22W-8Zr-3Mo).

[0062] Comparative Example 1

[0063] Comparative Example 1 provides a pure titanium.

[0064] Comparative Example 2

[0065] Comparative Example 2 provides a multi-element titanium alloy, the mass percentage of each element of which is shown in Table 1, and its preparation method is the same as that of Example 1.

[0066] Comparative Example 3

[0067] Comparative Example 3 provides a multi-element titanium alloy, the mass percentage of each element of which is shown in Table 1, and its preparation method is the same as that of Example 1.

[0068] Table 1. Elemental mass percentages of Examples 1-5 and Comparative Examples 1-3

[0069] titanium Tungsten zirconium molybdenum Example 1 71wt.% 18wt.% 8wt.% 3wt.% Example 2 71wt.% 22wt.% 4wt.% 3wt.% Example 3 66wt.% 25wt.% 4wt.% 5wt.% Example 4 70wt.% 22wt.% 5wt.% 3wt.% Example 5 67wt.% 22wt.% 8wt.% 3wt.% Comparative Example 1 100wt.% — — — Comparative Example 2 76wt.% 13wt.% 8wt.% 3wt.% Comparative Example 3 57wt.% 32wt.% 8wt.% 3wt.%

[0070] Performance testing

[0071] Test Method: Multiple tensile dog bone samples, with gauge dimensions of 12*4*1.5mm, were prepared from the original samples via wire EDM. Tensile tests (MTS E45.504) were performed at room temperature with a strain rate of 10. -3 s -1 The digital image correlation (DIC) instrument and its onboard video extensometer are synchronized with the tensile testing machine to directly capture stress-strain data at a frame rate of 1Hz during the tensile process, obtaining stress-strain curves. The yield strength, tensile strength, and plasticity of the alloy are obtained from the stress-strain curves.

[0072] X-ray impermeability: Obtained through theoretical calculations. The results are shown in Table 2.

[0073] X-ray impermeability = mass attenuation coefficient (Mc) alloy Alloy density (ρ)

[0074]

[0075] Mc is the mass decay coefficient of the alloy; u i : Linear decay coefficient of the element; c i It is the mass fraction of the element; ρ i It is elemental density.

[0076] Table 2 Examples 1-5 and Comparative Examples 1-3

[0077]

[0078] As can be seen from Table 2, the multi-component titanium alloys of Examples 1-5 of the present invention exhibit good high strength, high plasticity, and X-ray impermeability. Comparative Examples 1-3 show that pure titanium has poor X-ray impermeability, as well as poor strength and plasticity. When the W content is too low, the X-ray impermeability decreases significantly; however, when the W content is too high, the elongation decreases substantially.

[0079] The present invention has been described in detail above with reference to the embodiments of the present invention. However, the present invention is not limited to the above embodiments. Within the scope of knowledge possessed by those skilled in the art, various changes can be made without departing from the spirit of the present invention.

Claims

1. A multi-component titanium alloy, characterized in that, Includes the following components calculated as a percentage by mass: Tungsten 18-25%; Zirconium 4-8%; Molybdenum 2-5%; Balance titanium and unavoidable impurities; The multi-component titanium alloy is prepared by the following method: S1. Weigh tungsten, zirconium, molybdenum and titanium and melt them into alloy ingots; S2. The alloy ingot from step S1 is cold-rolled and deformed into a slab. S3. The plate is solution treated, and then quenched and cooled to room temperature; In step S2, the deformation amount of the cold rolling deformation is greater than 90%.

2. The multi-component titanium alloy according to claim 1, characterized in that, In step S3, the solution temperature of the solution treatment is 900℃~1200℃.

3. The multi-component titanium alloy according to claim 1, characterized in that, In step S3, the heat treatment time for the solution treatment is 5 min to 60 min.

4. The multi-component titanium alloy according to claim 1, characterized in that, In step S3, the cooling rate is 550℃ / s ~ 650℃ / s.

5. The multi-component titanium alloy according to claim 1, characterized in that, In step S1, the melting temperature is 3000℃~3200℃.

6. The multi-component titanium alloy according to claim 1, characterized in that, In step S1, the smelting apparatus is a non-consumable vacuum arc furnace.

7. The application of the multi-element titanium alloy according to any one of claims 1 to 6 in the fabrication of cardiovascular stents.

Images