Titanium-tantalum alloy component and preparation method and application thereof

Abstract

The invention provides a titanium-tantalum alloy component and a preparation method and application thereof. The preparation method of the titanium-tantalum alloy component comprises the steps that S1, titanium and tantalum are prepared into a titanium-tantalum alloy bar through smelting; s2, the titanium-tantalum alloy bar is subjected to gas atomization powder manufacturing or rotating electrode powder manufacturing under inert gas protection, and titanium-tantalum pre-alloyed powder is obtained; and S3, 3D printing is conducted on the titanium-tantalum pre-alloy powder, and the titanium-tantalum alloy component is obtained. According to the method, firstly, titanium and tantalum are smelted and evenly mixed, then gas atomization powder manufacturing or rotating electrode powder manufacturing is conducted, titanium powder and tantalum powder of the powder are evenly distributed, finally, 3D printing is conducted on the powder, and due to the fact that the size of a 3D printing molten pool is small, macrosegregation generated in a conventional preparation method can be effectively avoided; and finally, a titanium-tantalum alloy component which is fine and uniform in structure and good in alloy performance is obtained.

Description

Technical Field

[0001] The present invention relates to a method for preparing a titanium-tantalum alloy component, a titanium-tantalum alloy component obtained by the method for preparing the titanium-tantalum alloy component, and applications of the titanium-tantalum alloy component. Background Art

[0002] Titanium and titanium alloys have many advantages related to biological properties, such as low elastic modulus, good toughness, high strength, high specific strength, etc. Its dense oxide film can still exist stably in the body, has excellent corrosion resistance, wear resistance and excellent biocompatibility, and is the preferred alloy material for load-bearing restorations in interventional medicine and orthopedics.

[0003] With the vigorous development of biomedical materials, the demand for high-performance, low-cost and long-life biomedical materials is increasing rapidly. Titanium-tantalum alloy, as a new type of β-type titanium alloy, has excellent deep hardening ability. The addition of tantalum not only improves the bone compatibility of the material, enhances the strength and wear resistance of the titanium alloy, but also significantly reduces its elastic modulus, thereby improving the problem of high modulus of medical titanium alloys, reducing the adverse effects of implants on bones, and is lower in cost than pure tantalum.

[0004] The common preparation methods of titanium-tantalum alloy components are mainly prepared by smelting or powder metallurgy. However, during smelting, titanium-tantalum alloy faces serious defects such as component segregation and shrinkage defects due to the great difference in the melting points and densities of the two main elements. It is often necessary to increase multiple hot deformation and annealing treatments to partially eliminate the above defects, which makes it difficult to stably control the quality and performance of titanium-tantalum alloys, bringing many challenges to its preparation and application. In addition, the structure obtained by smelting is relatively coarse, which affects the performance of the alloy and limits its application in various fields. Powder metallurgy cannot obtain titanium-tantalum alloy samples with complex structures, and has large processing allowances, low material utilization, high mold costs, long production cycles, and high production costs. In powder metallurgy, powder needs to be prepared first, and the common preparation method of titanium-tantalum alloy pre-alloy powder is mainly to hydrogenate, crush, dehydrogenate and plasma spheroidize titanium-tantalum alloy ingots in sequence. However, on the one hand, this operation will result in a high oxygen content in the prepared titanium-tantalum alloy pre-alloy powder; on the other hand, since it needs to go through processes such as hydrogenation, mechanical crushing, dehydrogenation, and plasma spheroidization, the process is complicated and increases costs. Summary of the invention

[0005] The present invention aims to solve the problems in the prior art that the preparation and forming process of titanium-tantalum alloy pre-alloy powder is complicated, the obtained product has a coarse structure, low material utilization rate and difficulty in preparing complex parts, and provides a titanium-tantalum alloy component and its preparation method and application.

[0006] The technical method of the present invention is as follows:

[0007] A method for preparing a titanium-tantalum alloy component, the preparation method comprising: S1, preparing titanium and tantalum into titanium-tantalum alloy rods by smelting; S2, atomizing or rotating electrode powdering the titanium-tantalum alloy rods under the protection of an inert gas to obtain titanium-tantalum pre-alloyed powder; S3, 3D printing the titanium-tantalum pre-alloyed powder to obtain a titanium-tantalum alloy component.

[0008] The mass ratio of titanium to tantalum in step S1 is 5% to 95%: 5% to 95%.

[0009] In the step S1, the smelting step includes: B1, repeatedly smelting titanium blocks and tantalum blocks in a magnetic levitation furnace under the protection of inert gas to obtain titanium-tantalum alloy blocks; B2, smelting and cooling several titanium-tantalum alloy blocks obtained in the step B1 in a magnetic levitation furnace under the protection of inert gas to form ingots; B3, vacuum sintering the ingots to obtain titanium-tantalum alloy rods.

[0010] Specifically, in the step B1, the number of repeated smelting is more than 5 times, and the smelting temperature ranges from 1850°C to 2000°C.

[0011] Specifically, in step B3, the vacuum sintering temperature is 1600-1700° C., and the vacuum sintering time is more than 4 hours.

[0012] The 3D printing includes laser melting deposition (LMD) printing or selective laser melting (SLM) printing.

[0013] Specifically, the SLM printing steps include: using titanium alloy or pure titanium as a substrate, using 15 to 53 micron titanium-tantalum pre-alloy powder, and printing layer by layer according to a three-dimensional model of the part to obtain a titanium-tantalum alloy component.

[0014] Specifically, the LMD steps include: using titanium alloy or pure titanium as a substrate, using 53-150 micron titanium-tantalum pre-alloy powder, and printing layer by layer according to a three-dimensional model of the part to obtain a titanium-tantalum alloy component.

[0015] The present invention also provides a titanium-tantalum alloy component, which is prepared by the above-mentioned method for preparing the titanium-tantalum alloy component.

[0016] The present invention also provides an application of a titanium-tantalum alloy component. The titanium-tantalum alloy component is prepared by the above-mentioned method for preparing the titanium-tantalum alloy component. The uses of the titanium-tantalum alloy component include being used as a biomedical material.

[0017] The beneficial effects of the present invention are:

[0018] 1) The present invention firstly smelts titanium and tantalum to uniformly mix the titanium and tantalum, then performs gas atomization powder making or rotary electrode powder making to uniformly distribute the titanium and tantalum powders of the powder, and finally uses 3D printing to print the powder. Since the size of the 3D printing molten pool is small, the macro segregation produced in the conventional preparation method can be effectively avoided, and finally a titanium-tantalum alloy component with fine and uniform structure and good alloy properties is obtained.

[0019] 2) The process for preparing titanium-tantalum alloy components of the present invention is simple and stable.

[0020] 3) The 3D printing technology of the present invention is used to prepare titanium-tantalum alloy components without the need for molds, with low material costs and high material utilization.

[0021] 4) The entire process of the titanium-tantalum pre-alloying of the present invention is carried out in an inert gas or vacuum, thereby ensuring that impurities such as oxygen in the powder can be effectively regulated according to the raw materials, thereby achieving precise control of the oxygen content in the alloy. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a scanning image of a titanium-tantalum alloy pre-alloy powder with a 95% tantalum content prepared for the rotating electrode in Example 1;

[0023] Figure 2 Energy spectrum of titanium-tantalum alloy pre-alloy powder with 95% tantalum content prepared for the rotating electrode in Example 1;

[0024] Figure 3 This is a scanning image of a titanium-tantalum alloy pre-alloy powder with a 5% tantalum content prepared by gas atomization in Example 2;

[0025] Figure 4 The energy spectrum of the titanium-tantalum alloy pre-alloyed powder with 5% tantalum content prepared by gas atomization in Example 2;

[0026] Figure 5 This is a picture of a single-walled sample of a titanium-tantalum alloy with a 95% tantalum content prepared by LMD in Example 3;

[0027] FIG6 is an EBSD image of a single-walled titanium-tantalum alloy sample with a 95% tantalum content prepared by LMD in Example 3 and its grain size distribution image; FIG6(a) is an EBSD image of a single-walled titanium-tantalum alloy sample with a 95% tantalum content prepared by LMD; FIG6(b) is a grain size distribution image of a single-walled titanium-tantalum alloy sample with a 95% tantalum content prepared by LMD;

[0028] Figure 7 This is a picture of a titanium-tantalum alloy cone cylinder sample with 80% tantalum content prepared by LMD in Example 4;

[0029] Figure 8 This is a picture of a titanium-tantalum alloy ring sample with a 60% tantalum content prepared by LMD in Example 5;

[0030] Fig. 9 This is a picture of a titanium-tantalum alloy rotating body sample with a 5% tantalum content prepared by LMD in Example 6;

[0031] Fig.10 This is a picture of a titanium-tantalum alloy cube sample with a 40% tantalum content prepared by SLM in Example 7. DETAILED DESCRIPTION

[0032] The technical solution of the present invention is described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0033] The present invention provides a method for preparing a titanium-tantalum alloy, the preparation method comprising:

[0034] S1. Prepare titanium and tantalum into titanium-tantalum alloy rods by smelting.

[0035] In one embodiment, the mass ratio of titanium to tantalum in step S1 is 5% to 95%: 5% to 95%. For example, the mass ratio of titanium to tantalum can be 10% to 80%: 20% to 90%, 30% to 60%: 40% to 70%. The mass ratio of titanium to tantalum used in the present invention is 5% to 95%: 5% to 95%, which has a wide range and can meet the needs of different application scenarios.

[0036] In one embodiment, titanium and tantalum may be in the form of wire or block. The present invention preferably uses a block, which is more convenient for operators.

[0037] In one embodiment, in step S1, the smelting step includes:

[0038] B1. In a magnetic levitation furnace, titanium blocks and tantalum blocks are repeatedly smelted under the protection of inert gas to obtain titanium-tantalum alloy blocks.

[0039] In one embodiment, in step B1, the number of repeated smelting is more than 5 times, and the smelting temperature ranges from 1850° C. to 2000° C., so as to achieve alloy uniformity while reducing the volatilization of Ti.

[0040] B2. In a magnetic suspension furnace, several titanium-tantalum alloy blocks obtained in step B1 are melted and cooled into ingots under the protection of inert gas.

[0041] Specifically, after smelting, the alloy is cooled in a water-cooled copper mold to form an ingot. Several titanium-tantalum alloy blocks are smelted to fuse them together to form a larger block for subsequent rod casting and sintering. Here, the smelting temperature ranges from 1850°C to 2000°C.

[0042] B3. The ingot is vacuum sintered to obtain a titanium-tantalum alloy rod.

[0043] In one embodiment, in step B3, the vacuum sintering temperature is 1600-1700° C., and the vacuum sintering time is more than 4 hours. For example, the temperature may be 1650° C. and the time may be 5 hours, 6 hours, 8 hours, or 10 hours.

[0044] During the sintering process, tantalum foil is laid between the surface of the blank and the furnace body.

[0045] S2. Atomizing or rotating electrode powdering the titanium-tantalum alloy rod under the protection of an inert gas to obtain titanium-tantalum pre-alloyed powder.

[0046] For example, gas atomization powder making can adopt electrode induction gas atomization method (EIGA). Rotating electrode powder making can adopt plasma rotating electrode powder making method.

[0047] S3. Perform 3D printing on the titanium-tantalum pre-alloy powder to obtain a titanium-tantalum alloy component.

[0048] In one embodiment, 3D printing includes SLM printing or LMD printing.

[0049] In one embodiment, the SLM steps include: using titanium alloy or pure titanium as a substrate, using 15 to 53 micron titanium-tantalum pre-alloy powder, and printing layer by layer according to a three-dimensional model of the part to obtain a titanium-tantalum alloy component.

[0050] Specifically, SLM printing can select titanium alloy (TC4, TA10, TA15, etc.) as the substrate. The substrate size is not limited according to the specific molding size, and the surface is flat and cleaned. The printing is carried out using a laser power of 150-250W, a scanning rate of 600-1000mm / s, a deviation of 0.06-0.12mm, and a layer thickness of 0.02-0.04mm.

[0051] In one embodiment, the LMD printing step includes: using titanium alloy or pure titanium as a substrate, using 53-150 micron titanium-tantalum pre-alloy powder, and printing layer by layer according to a three-dimensional model of the part to obtain a titanium-tantalum alloy component.

[0052] Specifically, LMD printing can select titanium alloy (TC4, TA10, TA15, etc.) as the substrate. The substrate size is not limited according to the specific molding size, and the surface is flat and cleaned. The printing is carried out using a laser power of 1000-1600W, a scanning rate of 400-700mm / min, an offset of 2-3mm, and a layer thickness of 0.6-0.8mm.

[0053] In one embodiment, the titanium-tantalum pre-alloy powder may be dried before printing. Drying may be performed by vacuum drying. The present invention does not specifically limit the model of the vacuum drying oven, and an instrument or device familiar to a person skilled in the art may be used. The drying temperature is 100 to 140° C. The drying time is 1 to 3 hours. For example, the drying temperature may be 110° C., 120° C., or 130° C. The drying time may be 2 hours.

[0054] The 3D printing preparation method of the present invention has the advantages of short preparation cycle, high material utilization rate, simple process, etc. At the same time, the 3D printing formability of the alloy and the performance of the alloy can be improved synchronously through the 3D printing process parameters, providing a theoretical and technical basis for the application of such alloys.

[0055] In one embodiment, the titanium-tantalum alloy component can also be cut to separate the substrate.

[0056] The present invention uses two methods, gas atomization and rotating electrode, to prepare titanium-tantalum pre-alloy powder with a tantalum content of 5%-95%, introduces 3D printing technology, and utilizes the advantages of near-net-shape forming, no mold required, and fine and uniform structure, to achieve rapid preparation of high-density titanium-tantalum alloy components with specific structures from two powders. This method reduces the difficulty of titanium-tantalum alloy processing, reduces processing allowance, saves production costs, and ultimately obtains a high-density and fine and uniform structure.

[0057] The present invention also provides an application of a titanium-tantalum alloy component. The titanium-tantalum alloy component is prepared by the above-mentioned method for preparing the titanium-tantalum alloy component. The uses of the titanium-tantalum alloy component include being used as a biomedical material.

[0058] Below in conjunction with specific embodiments, some embodiments of the present invention are described in detail. In the case of no conflict, the following embodiments and the features in the embodiments can be combined with each other. In the embodiments, if specific conditions are not specified, they are carried out according to normal conditions or the conditions recommended by the manufacturer. If the manufacturer is not specified for the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0059] Example 1 Preparation of a rotating electrode from titanium-tantalum alloy pre-alloy powder with 95% tantalum content

[0060] Step 1: Select high-purity titanium block and high-purity tantalum block, configure about 5 kg according to the mass ratio of Ti 5Ta 95, and repeatedly smelt them in a magnetic levitation furnace for more than 5 times to achieve alloy uniformity.

[0061] Step 2: Place the alloy blocks obtained in the previous step in the magnetic levitation furnace for smelting again. After smelting, cool the alloy in a water-cooled copper mold to form an ingot.

[0062] Step 3: Place the ingot in a vacuum sintering furnace and sinter at 1650°C for more than 4 hours, and lay tantalum foil between the surface of the blank and the furnace body.

[0063] Step 4: Process the sintered blank to obtain titanium-tantalum alloy rods, and then perform rotary electrode powder making. Figure 1 and Figure 2 shown.

[0064] Example 2 Preparation of 5% Tantalum Content Titanium-Tantalum Alloy Pre-alloyed Powder by Gas Atomization

[0065] Step 1: Select high-purity titanium blocks and high-purity tantalum blocks, configure about 5 kg according to the mass ratio of Ti 95Ta 5, and repeatedly smelt them in a magnetic levitation furnace for more than 5 times to achieve uniform alloy.

[0066] Step 2: Place the alloy blocks obtained in the previous step in the magnetic levitation furnace for smelting again. After smelting, cool the alloy in a water-cooled copper mold to form an ingot.

[0067] Step 3: Place the ingot in a vacuum sintering furnace and sinter at 1650°C for more than 4 hours, and lay tantalum foil between the surface of the blank and the furnace body.

[0068] Step 4: Process the sintered blank to obtain titanium-tantalum alloy rods, and then perform gas atomization powder making. Figure 3 and Figure 4 shown.

[0069] Example 3 Ti5Ta95 alloy LMD 3D printing

[0070] Using TC4 as the substrate, the titanium-tantalum alloy pre-alloyed powder in Example 1 was screened, and the powder of 53 to 150 μm was selected. After being placed in a vacuum drying oven at 120° C. for 2 h, it was printed layer by layer according to the three-dimensional model of the part to make a rough blank of a titanium-tantalum alloy single-wall part, such as Figure 5 As shown in Figure 6, the EBSD results show that the grain size of the printed titanium-tantalum alloy is about 43 microns, which belongs to a fine-grained structure; and the grain size is uniform.

[0071] Example 4 Ti20Ta80 alloy LMD 3D printing

[0072] Using TC4 as the substrate, the titanium-tantalum alloy pre-alloyed powder was screened, and the powder of 53 to 150 microns was selected. After being placed in a vacuum drying oven at 120°C for 2 hours, it was printed layer by layer according to the three-dimensional model of the part to make a rough blank of the titanium-tantalum alloy cone cylinder part layer by layer. The sample is as follows Figure 7 shown.

[0073] Example 5 Ti40Ta60 alloy LMD 3D printing

[0074] Using TC4 as the substrate, the titanium-tantalum alloy pre-alloy powder was screened, and the powder of 53 to 150 microns was selected. After being placed in a vacuum drying oven and dried at 120°C for 2 hours, the rough blank of the titanium-tantalum alloy circular ring part was printed layer by layer according to the three-dimensional model of the part. The rough blank of the part was separated from the substrate by wire cutting to obtain the titanium-tantalum alloy circular ring sample. The titanium-tantalum alloy circular ring sample is as follows. Figure 8 shown.

[0075] Example 6 Ti95Ta5 alloy LMD 3D printing

[0076] Using TC4 as the substrate, the titanium-tantalum alloy pre-alloy powder was screened, and the powder of 53-150 microns was selected. After being placed in a vacuum drying oven at 120°C for 2 hours, it was printed layer by layer according to the three-dimensional model of the part, and the rough blank of the titanium-tantalum alloy rotating body part was made layer by layer. The rough blank of the part was separated from the substrate by wire cutting to obtain the titanium-tantalum alloy rotating body sample. The titanium-tantalum alloy cone cylinder sample is as follows Fig. 9 shown.

[0077] Example 7 Ti60Ta40 alloy SLM 3D printing

[0078] Using pure titanium as the substrate, the titanium-tantalum alloy pre-alloyed powder was screened, and the powder of 15 to 53 microns was selected. After being placed in a vacuum drying oven at 120°C for 2 hours, it was printed layer by layer according to the three-dimensional model of the part, and a titanium-tantalum alloy cubic part rough blank was made layer by layer. The rough blank of the part was separated from the substrate by wire cutting to obtain a titanium-tantalum alloy cubic sample. Fig.10 shown; Fig.10 The horizontal and vertical values ​​are printing parameters.

[0079] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a titanium-tantalum alloy component, characterized in that: The preparation method comprises: S1. Preparing titanium and tantalum into titanium-tantalum alloy rods by smelting; S2, atomizing or rotating electrode powdering the titanium-tantalum alloy rod under the protection of an inert gas to obtain a titanium-tantalum pre-alloy powder; S3. Perform 3D printing on the titanium-tantalum pre-alloy powder to obtain a titanium-tantalum alloy component.

2. The preparation method according to claim 1, characterized in that: The mass ratio of titanium to tantalum in step S1 is 5% to 95%: 5% to 95%.

3. The preparation method according to claim 1, characterized in that: In the step S1, the smelting step includes: B1. In a magnetic suspension furnace, repeatedly smelt titanium blocks and tantalum blocks under the protection of inert gas to obtain titanium-tantalum alloy blocks; B2, in a magnetic suspension furnace, melting and cooling the titanium-tantalum alloy blocks obtained in step B1 into ingots under the protection of inert gas; B3. The ingot is vacuum sintered to obtain a titanium-tantalum alloy rod.

4. The preparation method according to claim 3, characterized in that: In the step B1, the number of repeated smelting is more than 5 times, and the smelting temperature ranges from 1850°C to 2000°C.

5. The preparation method according to claim 3, characterized in that: In the step B3, the vacuum sintering temperature is 1600-1700° C., and the vacuum sintering time is more than 4 hours.

6. The preparation method according to claim 1, characterized in that: The 3D printing includes laser melting deposition printing or selective laser melting printing.

7. The preparation method according to claim 6, characterized in that: The steps of selective laser melting printing include: Using titanium alloy or pure titanium as the substrate, and using 15 to 53 micron titanium-tantalum pre-alloy powder, the parts are printed layer by layer according to the three-dimensional model to obtain titanium-tantalum alloy components.

8. The preparation method according to claim 6, characterized in that: The laser melting deposition printing step includes: using titanium alloy or pure titanium as a substrate, using 53-150 micron titanium-tantalum pre-alloy powder, and printing layer by layer according to the three-dimensional model of the part to obtain a titanium-tantalum alloy component.

9. A titanium-tantalum alloy component, characterized in that: The titanium-tantalum alloy component is prepared by the method for preparing a titanium-tantalum alloy component according to any one of claims 1 to 8.

10. An application of a titanium-tantalum alloy component, characterized in that: The titanium-tantalum alloy component is prepared by the method for preparing a titanium-tantalum alloy component according to any one of claims 1 to 8, and the use of the titanium-tantalum alloy component includes being used as a biomedical material.

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