A method for preparing a homogeneous titanium-tantalum alloy ingot based on a titanium-tantalum composite precursor

Abstract

The application discloses a method for preparing homogeneous titanium-tantalum alloy ingot based on a titanium-tantalum composite precursor, and the method comprises the following steps: firstly, placing sponge titanium in a slot of a magnetron sputtering device and taking the sponge titanium as an anode, and taking a metal tantalum target as a cathode to perform magnetron sputtering to obtain a titanium-tantalum composite precursor; and secondly, mixing the sponge titanium and the titanium-tantalum composite precursor, pressing the mixture into a billet, welding the billet into a consumable electrode, and performing vacuum arc melting to obtain a homogeneous titanium-tantalum alloy ingot. The method adopts the magnetron sputtering method, so that tantalum atoms are uniformly and firmly attached to the sponge titanium to prepare the titanium-tantalum composite precursor, the distribution uniformity of the tantalum element is improved, the high-melting-point tantalum element inclusions are effectively avoided, the preparation of the high-homogeneous titanium-tantalum alloy ingot is realized, the titanium-tantalum alloy ingot production process is effectively simplified, the ingot melting frequency is reduced, and the production efficiency and the yield of the homogeneous titanium-tantalum alloy ingot are improved, and the production cost is reduced.

Description

Technical Field

[0001] This invention belongs to the field of titanium alloy preparation technology, specifically relating to a method for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors. Background Technology

[0002] Titanium-tantalum alloys are binary alloys composed of titanium and tantalum, with tantalum content ranging from 0.5% to 10% by mass, the remainder being titanium and unavoidable impurities. Due to their excellent resistance to nitric acid corrosion, titanium-tantalum alloys can be used in the manufacture of nuclear chemical containers and acid-resistant containers. However, because tantalum is a high-melting-point, high-density metal with significantly different properties from titanium, high-density tantalum inclusions are easily generated during the preparation of titanium-tantalum alloys, resulting in inhomogeneity in the composition, microstructure, and properties of the ingot. To address this issue, two common approaches are currently employed: one involves mixing tantalum powder and titanium powder (or sponge titanium) to prepare a consumable electrode, followed by multiple (at least three) vacuum arc melting processes to suppress tantalum infusible block defects and improve ingot uniformity; the other involves preparing a Ti-Ta master alloy using a mixture of tantalum and titanium powder, then machining the uniformly melted, lower-melting-point Ti-Ta master alloy into metal chips. These chips are then mixed with titanium powder (or sponge titanium) to prepare a consumable electrode, and finally, a well-uniform titanium-tantalum alloy ingot is prepared through vacuum arc melting. Currently, there are no reports of using titanium-tantalum composite precursors to prepare titanium-tantalum alloy ingots. Summary of the Invention

[0003] The technical problem to be solved by this invention is to address the shortcomings of the prior art by providing a method for preparing homogeneous titanium-tantalum alloy ingots based on a titanium-tantalum composite precursor. This method employs magnetron sputtering to uniformly and firmly attach tantalum atoms onto sponge titanium to prepare the titanium-tantalum composite precursor. The precursor is then mixed with sponge titanium and subjected to vacuum arc melting, which improves the uniformity of tantalum element distribution and effectively avoids the inclusion of high-melting-point tantalum elements. This achieves the preparation of highly homogeneous titanium-tantalum alloy ingots and solves the metallurgical problems caused by existing tantalum powder addition methods, such as uneven distribution of high-melting-point tantalum components and difficulties in alloying.

[0004] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is as follows: a method for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors, characterized in that the method includes the following steps:

[0005] Step 1: Preparation of titanium-tantalum composite precursor: Sponge titanium is placed in the tank of a magnetron sputtering equipment and used as the anode as a whole. A tantalum metal target is used as the cathode. After setting the bias voltage, power and time parameters, magnetron sputtering is performed so that the sputtered tantalum metal atoms are uniformly attached to the surface of the sponge titanium to obtain the titanium-tantalum composite precursor.

[0006] Step 2, Preparation of titanium-tantalum alloy ingot: Sponge titanium and the titanium-tantalum composite precursor obtained in Step 1 are placed in a mixer for mixing. After mixing, the material is pressed into a billet using a cold isostatic press. The billet is then welded to form a consumable electrode and placed in a vacuum consumable arc furnace for vacuum arc melting to obtain a homogeneous titanium-tantalum alloy ingot.

[0007] Typically, the mass of tantalum in the titanium-tantalum composite precursor prepared by this invention is determined by the difference between the mass of the titanium-tantalum composite precursor and the mass of sponge titanium before magnetron sputtering.

[0008] The method for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors is characterized in that the mass purity of the tantalum metal target material in step one is above 99.99%.

[0009] The method for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors is characterized in that the bias voltage of magnetron sputtering in step one is 10V to 200V, the power is 120W to 350W, and the time is 10min to 300min.

[0010] The method described above for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors is characterized in that, in step two, the mass content of tantalum in the homogeneous titanium-tantalum alloy ingot is 0.5% to 10%, with the remainder being titanium and unavoidable impurities. The homogeneous titanium-tantalum alloy ingots prepared by this invention meet the requirements of commonly used titanium-tantalum alloys.

[0011] The method for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors, as described above, is characterized in that the pressing pressure in step two is 15 MPa to 60 MPa, and the holding time is 1 s to 60 s. These pressing process parameters ensure that the billet has sufficient strength.

[0012] The method described above for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors is characterized in that, in step two, the vacuum arc melting process is carried out under the following conditions: a vacuum degree below 5 Pa, a leakage rate below 1 Pa / min, a melting voltage of 25 V to 36 V, a melting current of 5 kA to 10 kA, and a cooling time of not less than 2.5 h after melting. These vacuum arc melting process parameters ensure sufficient alloying of titanium and tantalum.

[0013] Compared with the prior art, the present invention has the following advantages:

[0014] 1. This invention uses magnetron sputtering to prepare titanium-tantalum composite precursors, achieving uniform adhesion of tantalum atoms on sponge titanium. Combined with vacuum arc melting, a homogeneous titanium-tantalum alloy ingot is obtained. This effectively solves the metallurgical problems caused by the existing tantalum powder addition method, such as uneven distribution of high-melting-point tantalum components and difficulty in alloying. It solves the problem of poor uniformity of titanium-tantalum alloy ingots and easy formation of tantalum infusible blocks from the source of raw materials.

[0015] 2. Compared with the direct mixing of tantalum powder and titanium powder (or sponge titanium), the present invention uses a titanium-tantalum composite precursor to prepare titanium-tantalum alloy ingots. Since the tantalum element in the titanium-tantalum composite precursor is uniformly attached to the sponge titanium and the bonding force between the two is strong, the tantalum component is not easy to fall off and be unevenly distributed, effectively avoiding high-density tantalum inclusions caused by uneven dispersion of tantalum powder.

[0016] 3. This invention uses titanium-tantalum composite precursors to prepare titanium-tantalum alloy ingots, which effectively simplifies the titanium-tantalum alloy ingot production process, reduces the number of ingot melting times, improves the production efficiency and yield of homogeneous titanium-tantalum alloy ingots, and reduces production costs.

[0017] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description

[0018] Figure 1 This is a physical image of the titanium-tantalum composite precursor prepared in Example 1 of the present invention.

[0019] Figure 2 This is a photograph of the blank formed by pressing the titanium-tantalum composite precursor and sponge titanium in Example 1 of the present invention.

[0020] Figure 3 This is a physical image of a consumable electrode made by welding a blank in Embodiment 1 of the present invention.

[0021] Figure 4 Metallographic image of the homogeneous titanium-tantalum alloy ingot prepared in Example 1 of the present invention.

[0022] Figure 5a This is a distribution diagram of Ti element in the homogeneous titanium-tantalum alloy ingot prepared in Example 1 of the present invention.

[0023] Figure 5b This is a distribution diagram of Ta element in the homogeneous titanium-tantalum alloy ingot prepared in Example 1 of the present invention. Detailed Implementation

[0024] Example 1

[0025] This embodiment includes the following steps:

[0026] Step 1: Preparation of the titanium-tantalum composite precursor: 300 kg of sponge titanium was placed in batches in a magnetron sputtering tank and used as the anode. A 99.995% pure tantalum target was used as the cathode. Magnetron sputtering was performed with a bias voltage of 10V, a power of 240W, and a time parameter of 60 min, ensuring that the sputtered tantalum atoms uniformly adhered to the surface of the sponge titanium, resulting in 312.2 kg of titanium-tantalum composite precursor. Figure 1 As shown; the sponge titanium conforms to the national standard GB / T 2524-2019 "Sponge Titanium";

[0027] Step 2, Titanium-Tantalum Alloy Ingot Preparation: 2125 kg of sponge titanium and 312.2 kg of titanium-tantalum composite precursor obtained in Step 1 were mixed in a V-type mixer. After mixing, the material was pressed into a billet using a cold isostatic press. Figure 2 As shown, the pressing pressure is 56 MPa, the holding time is 5 seconds, and then the blank is welded to form a consumable electrode, as shown. Figure 3 As shown, the material is placed in a vacuum arc melting furnace for vacuum arc melting. The vacuum degree of the vacuum arc melting is 2.8 Pa, the leakage rate is 0.8 Pa / min, the melting voltage is 25 V to 29 V, the melting current is 8 kA, and the cooling time after melting is 3 h, to obtain a homogeneous titanium-tantalum alloy ingot. The mass content of tantalum in the homogeneous titanium-tantalum alloy ingot is 0.5%, and the remainder is titanium and unavoidable impurities.

[0028] Figure 4 The metallographic image of the homogeneous titanium-tantalum alloy ingot prepared in this embodiment is shown below. Figure 4 It can be seen that the microstructure of the homogeneous titanium-tantalum alloy ingot exhibits the typical equiaxed crystal and grain boundary microstructure characteristics of titanium-tantalum alloy ingots, and no tantalum infusible blocks are observed.

[0029] Figure 5a and Figure 5b These are the element distribution diagrams of Ti and Ta in the homogeneous titanium-tantalum alloy ingot prepared in this embodiment. Figure 5a and Figure 5b The uniform distribution of Ti and Ta elements in the titanium-tantalum alloy ingot indicates that the present invention has achieved the preparation of a homogeneous titanium-tantalum alloy ingot.

[0030] Example 2

[0031] This embodiment includes the following steps:

[0032] Step 1: Preparation of Titanium-Tantalum Composite Precursor: 630 kg of sponge titanium was placed in batches in the magnetron sputtering tank and used as the anode. A 99.995% pure tantalum metal target was used as the cathode. After setting the bias voltage to 150V, the power to 350W, and the time parameter to 10min, magnetron sputtering was performed to ensure that the sputtered tantalum metal atoms were uniformly attached to the surface of the sponge titanium, resulting in 689.4 kg of titanium-tantalum composite precursor. The sponge titanium conforms to the national standard GB / T 2524-2019 "Sponge Titanium".

[0033] Step 2: Preparation of Titanium-Tantalum Alloy Ingots: 288 kg of sponge titanium and 689.4 kg of titanium-tantalum composite precursor obtained in Step 1 were mixed in a V-type mixer. After mixing, the material was pressed into a billet using a cold isostatic press at a pressure of 60 MPa and a holding time of 1 s. The billet was then welded to form a consumable electrode and placed in a vacuum arc melting furnace for vacuum arc melting. The vacuum degree of the vacuum arc melting was 3 Pa, the leakage rate was 0.9 Pa / min, the melting voltage was 30 V to 36 V, the melting current was 10 kA, and the cooling time after melting was 3 h, resulting in a homogeneous titanium-tantalum alloy ingot. The mass content of tantalum in the homogeneous titanium-tantalum alloy ingot was 6%, with the remainder being titanium and unavoidable impurities.

[0034] Example 3

[0035] This embodiment includes the following steps:

[0036] Step 1: Preparation of Titanium-Tantalum Composite Precursor: 520 kg of sponge titanium was placed in batches in the magnetron sputtering tank and used as the anode. A 99.995% pure tantalum metal target was used as the cathode. After setting the bias voltage to 200V, the power to 120W, and the time parameter to 300 min, magnetron sputtering was performed to ensure that the sputtered tantalum metal atoms were uniformly attached to the surface of the sponge titanium, resulting in 608.9 kg of titanium-tantalum composite precursor. The sponge titanium conforms to the national standard GB / T 2524-2019 "Sponge Titanium".

[0037] Step 2: Preparation of Titanium-Tantalum Alloy Ingots: 280 kg of sponge titanium and 608.9 kg of titanium-tantalum composite precursor obtained in Step 1 were mixed in a V-type mixer. After mixing, the material was pressed into a billet using a cold isostatic press at a pressure of 15 MPa and a holding time of 60 s. The billet was then welded to form a consumable electrode and placed in a vacuum arc melting furnace for vacuum arc melting. The vacuum degree of the vacuum arc melting was 3.1 Pa, the leakage rate was 0.9 Pa / min, the melting voltage was 25 V to 30 V, the melting current was 5 kA, and the cooling time after melting was 3 h, resulting in a homogeneous titanium-tantalum alloy ingot. The mass content of tantalum in the homogeneous titanium-tantalum alloy ingot was 10%, with the remainder being titanium and unavoidable impurities.

[0038] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention in any way. Any simple modifications, alterations, and equivalent changes made to the above embodiments based on the inventive essence shall still fall within the protection scope of the present invention.

Claims

1. A method for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors, characterized in that, The method includes the following steps: Step 1: Preparation of titanium-tantalum composite precursor: Sponge titanium is placed in the tank of a magnetron sputtering equipment and used as the anode as a whole. A tantalum metal target is used as the cathode. After setting the bias voltage, power and time parameters, magnetron sputtering is performed so that the sputtered tantalum metal atoms are uniformly attached to the surface of the sponge titanium to obtain the titanium-tantalum composite precursor. Step 2, Preparation of Titanium-Tantalum Alloy Ingot: Sponge titanium and the titanium-tantalum composite precursor obtained in Step 1 are mixed in a mixer. After mixing, the material is pressed into a billet using a cold isostatic press. The billet is then welded to form a consumable electrode, which is then placed in a vacuum arc melting furnace for vacuum arc melting to obtain a homogeneous titanium-tantalum alloy ingot. The mass content of tantalum in the homogeneous titanium-tantalum alloy ingot is 0.5%~10%, with the remainder being titanium and unavoidable impurities.

2. The method for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors according to claim 1, characterized in that, The tantalum metal target material mentioned in step one has a purity of 99.99% or higher.

3. The method for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors according to claim 1, characterized in that, The bias voltage of the magnetron sputtering in step one is 10V~200V, the power is 120W~350W, and the time is 10min~300min.

4. The method for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors according to claim 1, characterized in that, The pressing pressure in step two is 15MPa~60MPa, and the holding time is 1s~60s.

5. The method for preparing homogeneous titanium-tantalum alloy ingots based on titanium-tantalum composite precursors according to claim 1, characterized in that, In step two, the vacuum degree of vacuum arc melting is below 5 Pa, the leakage rate is below 1 Pa / min, the melting voltage is 25V~36V, the melting current is 5kA~10kA, and the cooling time after melting is not less than 2.5h.

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