CN112126819A - Smelting method of titanium alloy material with high niobium content - Google Patents
Smelting method of titanium alloy material with high niobium content Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C14/00—Alloys based on titanium
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C22C1/10—Alloys containing non-metals
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
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Abstract
The invention relates to a smelting method of a titanium alloy material with high niobium content, which comprises the following steps: the method comprises the steps of proportioning titanium alloy with high niobium content according to components except niobium, pressing the titanium alloy on a hydraulic press to form an electrode, bundling or welding the electrode with a niobium plate, and smelting the combined electrode for three times by sequentially adopting a vacuum consumable arc furnace, a shell furnace and a vacuum consumable arc furnace to finally obtain a titanium alloy ingot with uniform components and high niobium content. In the electrode preparation process before smelting, the niobium alloy element is added in a mode of binding and welding the niobium plate strips with the consumable electrode, and a mode of one-time vacuum shell-type furnace smelting is adopted, so that the situations that the intermediate alloy and titanium sponge account for too large ratio, the finally pressed consumable electrode has insufficient strength, the intermediate alloy is easy to spill or fall in the smelting process, and the inclusion, segregation or uneven smelting of high-melting-point metal is formed can be effectively avoided.
Description
Technical Field
The invention relates to a method for smelting a titanium alloy material with high niobium content, and belongs to the technical field of titanium alloy material preparation.
Background
Compared with traditional medical metal materials such as stainless steel, cobalt-chromium-molybdenum alloy and the like, titanium and titanium alloy gradually become preferred materials in medical fields such as orthopedic surgery, implantation, oral repair and the like due to good comprehensive mechanical properties, corrosion resistance and excellent biocompatibility. In recent years, with the continuous development of biomedical titanium and titanium alloys, high-strength novel medical titanium alloys containing non-toxic elements, better biocompatibility and lower elastic modulus are developed and researched to meet the clinical requirements on implants, and become the main research target of the third generation of biomedical titanium alloy materials.
In the early 90 s, nontoxic elements such as Nb, Ta, Zr, Mo and Sn are selected to replace V and A1 in the United states and Japan, and a series of nontoxic medical beta-type titanium alloys with low elastic modulus are developed. The alloys developed in the united states are mainly: ti-13Nb-13Zr, Ti-12Mo-6Zr-2Fe (TMZF), Ti-15Mo, Ti-35Nb-5Ta-7Zr (TNTZ), etc. The alloys developed in japan are mainly: ti-29Nb-13Ta-4.6Zr, Ti-15Zr-4Nb-2Ta-0.2Pd and Ti-15Sn-4Nb-2Ta-0.2Pd, etc. Compared with the first generation and the second generation medical titanium alloys, the corrosion resistance and the biocompatibility of the novel beta-type titanium alloy are obviously improved, and the elastic modulus is reduced by 30-50 GPa, and is probably in the range of 55-85 GPa. From 2001 + 2005, the most representative of beta-type biological titanium alloys were Ti-24Nb-4Zr-7.9Sn (Ti2448) developed by the institute of metals of Chinese academy of sciences and Ti- (15-25) Nb- (3) Mo- (3-5) Zr (TLE) and Ti- (15-25) Nb- (3-6) Mo- (3-5) Zr- (1-2) Sn (TLM) beta-type titanium alloys developed by the institute of nonferrous metals in northwest China. The TLM and TLE alloy have the strength of 580-1000 MPa and the elastic modulus of 50-90 GPa. The Ti2448 alloy has lower elastic modulus and good elasticity, and is suitable for manufacturing elastic bone plates and dynamic fixers. Research and development of a novel beta type titanium alloy biomedical material with adjustable modulus, high strength and multifunctional application and a matched processing technology become an important direction for development of medical titanium alloy in the future. From the development process of the biomedical titanium alloy, the new generation biomedical titanium alloy is designed by adding high niobium content. Aiming at the titanium alloy with high niobium content, in the process of vacuum consumable arc melting of an industrial ingot, when the content of Nb element added in the titanium alloy reaches 10-40 percent in percentage by weight, the Ti-Nb intermediate alloy and part of Ti-Mo and Ti-Sn intermediate alloy ingredients required by the alloy melting exceed more than 60 percent, so that the addition amount of sponge titanium is small, the condition of large addition amount of intermediate alloy leads to insufficient strength of a final pressed consumable electrode, the intermediate alloy is easy to spill or fall in the melting process, the condition of inclusion, segregation or uneven melting of high-melting-point metal is caused, and the metallurgical quality of the titanium alloy ingot is seriously influenced.
Disclosure of Invention
The invention aims to avoid and overcome the hidden danger and the problem in the smelting process and provide a smelting method suitable for a titanium alloy material with high niobium content, thereby effectively reducing the difficulty of smelting the titanium alloy with high niobium content in a vacuum consumable electro-arc furnace and further improving the uniformity of the components of a titanium alloy ingot with high niobium content.
The purpose of the invention is solved by the following technical scheme:
the smelting method provided by the invention is that certain titanium alloy with high niobium content is firstly mixed according to the components except niobium element, and is pressed into an electrode on a hydraulic press and then bundled or welded with a niobium plate strip, and then the combined electrode is put into a vacuum consumable arc furnace and a vacuum shell furnace for vacuum consumable arc smelting for multiple times, and finally, a titanium alloy ingot with uniform components and high niobium content is obtained.
Further, the smelting method of the titanium alloy with high niobium content specifically comprises the following steps:
the method comprises the following steps: proportioning and pressing
Selecting corresponding scrap-shaped, granular or block-shaped intermediate alloys such as Ti-Mo, Ti-Ta and Ti-Sn according to the mass percentage of each component for proportioning, uniformly mixing the intermediate alloys with sponge titanium and sponge zirconium and pressing the intermediate alloys into block-shaped electrode blocks;
step two: electrode preparation
Assembling and welding the pressed electrode blocks into strip electrodes in a head-to-tail connection mode, and uniformly binding or welding pre-cut niobium plate strips at the periphery of the electrode strips at certain intervals to form a final consumable electrode;
step three: one-time smelting
Taking the assembled and welded strip-shaped electrode as a consumable electrode to carry out primary smelting in a vacuum consumable electric arc furnace to obtain a primary ingot;
step four: secondary smelting
Carrying out secondary smelting on the primary ingot serving as a consumable electrode in a shell type furnace to obtain a secondary ingot;
step five: three-time smelting
And (3) carrying out tertiary smelting on the secondary ingot as a consumable electrode in a vacuum consumable arc furnace, and finally cooling the secondary ingot in the furnace to below 200 ℃ to obtain a cylindrical finished ingot with a certain diameter and height.
Further, in the step one, the other alloy elements are Mo, Ta, Zr and Sn, and the intermediate alloy is one or more of Ti-Mo, Ti-Ta and Ti-Sn, wherein: ti is sponge Ti and TiO of zero grade2Adding Zr in the form of industrial sponge Zr, adding high-melting-point elements Mo and Ta in the form of Ti-32Mo and Ti-Ta intermediate alloy, adding volatile element Sn in the form of Ti-80Sn intermediate alloy, and making the oxygen content in the alloy pass through TiO2The content of (c) is controlled.
Further, in the second step, the electrode welding adopts vacuum argon arc welding, and the welding vacuum is less than 8 Pa.
And further, step three, carrying out primary vacuum consumable arc melting on the alloy, wherein the melting current is 1.5-10KA, the melting voltage is 26-36V, and the melting specification is phi 150-phi 440 mm.
And step four, smelting the alloy in a secondary shell type furnace, wherein the smelting current is 9.5-40KA, the smelting voltage is 32-48V, and the smelting specification phi is 220-phi 440 mm.
And further, step five, carrying out three times of vacuum consumable arc melting on the alloy, wherein the melting current is 8.0-25KA, the melting voltage is 33-38V, and the melting specification is phi 220-phi 620 mm.
Further, in the third step, the fourth step and the fifth step, the vacuum degree in the furnace is less than 6.77Pa during smelting.
Further, the sequence of step four and step five may be changed.
Further, the alloy finished ingot obtained in the fifth step needs to be placed into a resistance furnace for homogenization annealing, wherein the homogenization annealing temperature is 800-1000 ℃, and the time is 6-8 hours.
The invention has the following advantages and beneficial effects:
the invention adopts the steps of firstly batching the titanium alloy with high niobium content according to the components except niobium element, pressing an electrode, bundling or welding the electrode with a niobium plate strip to form a new electrode, and finally, carrying out multiple times of vacuum consumable melting on the combined new electrode in a mode of combining a vacuum consumable arc furnace with a shell furnace to obtain the titanium alloy ingot casting with uniform components.
The invention can effectively solve the problem of smelting the titanium alloy ingots with high niobium content, and provides a suitable multifunctional titanium alloy ingot smelting method.
The method can avoid the situations that the consumable electrode strength is insufficient due to the fact that excessive intermediate alloy is directly added in the traditional method, or the intermediate alloy is easy to spill or fall off during the smelting process, so that normal smelting cannot be carried out, or the inclusion, segregation and non-uniformity of high-melting-point metal occur, and meanwhile, a shell-type furnace smelting is adopted for once, so that an ingot casting molten pool can be effectively and uniformly smelted, high-melting-point elements in the ingot are fully homogenized, and the inclusion and segregation of the high-melting-point elements are further avoided.
The method can effectively reduce the difficulty of smelting the titanium alloy with high niobium content in the vacuum consumable electrode arc furnace, and further improve the metallurgical quality of the titanium alloy ingot with high niobium content, thereby bringing remarkable economic benefit.
Detailed Description
The invention relates to a method for smelting a titanium alloy with high niobium content, which is characterized in that niobium is added in a niobium slab form to prepare a combined consumable electrode, and a finished cast ingot is obtained by three times of smelting in a vacuum consumable arc furnace, a shell furnace and a vacuum consumable arc furnace, and can be effectively suitable for smelting cast ingots of multifunctional titanium alloys with high niobium content in the titanium alloy, wherein the niobium content in the titanium alloy is required to be 10-40% by weight.
The invention is described in further detail below by means of specific examples:
example 1:
the preparation method of the present invention is described by taking Ti-19Nb- (0.5-2%) Mo- (3-5%) Zr- (7-9%) Sn- (0.1-0.3%) O as an example.
Proportioning and pressing
Sponge titanium, sponge zirconium, intermediate alloy of Ti-32Mo, Ti-80Sn and the like are used as raw materials, and the raw materials comprise 4 percent of sponge zirconium, 32 percent of Ti-Mo, 80 percent of Ti-80 Sn: % of the mixture was 200kg and pressed by an oil press into electrode blocks weighing 5 kg.
Electrode preparation
Assembling and welding the pressed electrode blocks into long strip electrodes in a head-to-tail connection mode, and uniformly welding pre-cut niobium plate strips (19 wt%) around the long strip electrodes to form final consumable electrodes; the welding vacuum is less than 8 Pa.
Ingot melting
Taking the assembled and welded strip-shaped electrode as a consumable electrode to carry out primary smelting in a vacuum consumable electric arc furnace to obtain a primary ingot, wherein the smelting current is controlled to be 1.5-3.0KA, and the smelting voltage is 26-30W; carrying out secondary smelting on the primary ingot serving as a consumable electrode in a shell type furnace to obtain a secondary ingot, wherein the smelting current is controlled to be 9.5-12KA, and the smelting voltage is 32-36V; and further carrying out tertiary smelting on the secondary ingot as a consumable electrode in a vacuum consumable arc furnace to obtain a finished ingot, wherein the smelting current is controlled to be 8.0-9.0KA, and the smelting voltage is controlled to be 33-37V.
Cooling down
And cooling the ingot after the smelting to below 200 ℃ to discharge, and finally obtaining the required cylindrical finished ingot.
After the prepared product is subjected to lathe flat head facing and peeling, block-shaped and chip-shaped samples are respectively taken from the head and the bottom of the cast ingot and the upper, middle and lower positions of the cast ingot for component analysis, and the component analysis result of the niobium content is shown in table 1:
the Ti-19Nb- (0.5-2%) Mo- (3-5%) Zr- (7-9%) Sn- (0.1-0.3%) O alloy niobium content (%)
| Sampling site | Upper part | Middle part | Lower part | Head center | Head 1/2 | Bottom center | Bottom 1/2 |
| Nb content (wt%) | 18.56 | 18.91 | 19.03 | 17.49 | 18.59 | 18.48 | 18.73 |
Example 2
The preparation method of the invention is illustrated by taking Ti-24Nb-4Zr-7.9Sn as an example.
1) Proportioning and pressing
Sponge titanium, sponge zirconium and Ti-80Sn intermediate alloy are used as raw materials, and the raw materials comprise, by weight, 4% of sponge zirconium, Ti-80 Sn: % of the mixture was 200kg and pressed by an oil press into electrode blocks weighing 5 kg.
2) Electrode preparation
Assembling and welding the pressed electrode blocks into long strip electrodes in a head-to-tail connection mode, and uniformly welding pre-cut niobium plate strips (with the weight of 24%) around the long strip electrodes to form final consumable electrodes; the welding vacuum is less than 8 Pa.
3) Ingot melting
Taking the assembled and welded strip-shaped electrode as a consumable electrode to carry out primary smelting in a vacuum consumable electric arc furnace to obtain a primary ingot, wherein the smelting current is controlled to be 1.5-3.0KA, and the smelting voltage is 26-30W; carrying out secondary smelting on the primary ingot serving as a consumable electrode in a shell type furnace to obtain a secondary ingot, wherein the smelting current is controlled to be 9.5-12KA, and the smelting voltage is 32-36V; and further carrying out tertiary smelting on the secondary ingot as a consumable electrode in a vacuum consumable arc furnace to obtain a finished ingot, wherein the smelting current is controlled to be 8.0-9.0KA, and the smelting voltage is controlled to be 33-37V.
4) Cooling down
And cooling the ingot after the smelting to below 200 ℃ to discharge, and finally obtaining the required cylindrical finished ingot.
After the prepared product is subjected to lathe flat head facing and peeling, block-shaped and chip-shaped samples are respectively taken from the head and the bottom of the cast ingot and the upper, middle and lower positions of the cast ingot for component analysis, and the component analysis result of the niobium content is shown in table 2:
ti-24Nb-4Zr-7.9Sn alloy prepared in Table 2 has a niobium content (%)
| Sampling site | Upper part | Middle part | Lower part | Head center | Head 1/2 | Bottom center | Bottom 1/2 |
| Nb content (wt%) | 24.09 | 24.22 | 24.44 | 23.67 | 24.06 | 23.51 | 23.25 |
The alloy finished ingot can be subjected to forging, rolling and other processing processes according to a common beta titanium alloy processing method, and products such as alloy plates, bars, forgings and the like suitable for the medical industry are prepared.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The smelting method of the titanium alloy material with high niobium content is characterized by comprising the following steps: the method comprises the steps of proportioning titanium alloy with high niobium content according to components except niobium, pressing the titanium alloy on a hydraulic press to form an electrode, bundling or welding the electrode with a niobium plate, and smelting the combined electrode for three times by sequentially adopting a vacuum consumable arc furnace, a shell furnace and a vacuum consumable arc furnace to finally obtain a titanium alloy ingot with uniform components and high niobium content.
2. The method for smelting the titanium alloy material with the high niobium content as claimed in claim 1, wherein the method comprises the following steps:
the method comprises the following steps: proportioning and pressing
Selecting corresponding scrap-shaped, granular or block-shaped intermediate alloy for proportioning according to the mass percentage of each component of other alloy elements except niobium in the titanium alloy with high niobium content, uniformly mixing the intermediate alloy with titanium sponge and zirconium sponge, and pressing the intermediate alloy into a block-shaped electrode block;
step two: electrode preparation
Assembling and welding the pressed electrode blocks into strip electrodes in a head-to-tail connection mode, and uniformly binding or welding pre-cut niobium plate strips at the periphery of the electrode strips at certain intervals to form a final consumable electrode;
step three: one-time smelting
Taking the assembled and welded strip-shaped electrode as a consumable electrode to carry out primary smelting in a vacuum consumable electric arc furnace to obtain a primary ingot;
step four: secondary smelting
Carrying out secondary smelting on the primary ingot serving as a consumable electrode in a shell type furnace to obtain a secondary ingot;
step five: three-time smelting
And (3) carrying out tertiary smelting on the secondary ingot as a consumable electrode in a vacuum consumable arc furnace, and finally cooling the secondary ingot in the furnace to below 200 ℃ to obtain a cylindrical finished ingot with a certain diameter and height.
3. The titanium alloy material with high niobium content as claimed in claim 2The smelting method is characterized in that in the step one, other alloy elements comprise but are not limited to Mo, Ta, Zr and Sn, and the intermediate alloy comprises but is not limited to Ti-Mo, Ti-Ta and Ti-Sn, wherein: ti is sponge Ti and TiO of zero grade2Adding Zr in the form of industrial sponge Zr, adding high-melting-point elements Mo and Ta in the form of Ti-32Mo and Ti-Ta intermediate alloy, adding volatile element Sn in the form of Ti-80Sn intermediate alloy, and making the oxygen content in the alloy pass through TiO2The content of (c) is controlled.
4. The method for smelting the titanium alloy material with the high niobium content as claimed in claim 2, wherein in the second step, the electrode welding adopts vacuum argon arc welding, and the welding vacuum is less than 8 Pa.
5. The method for smelting the titanium alloy material with the high niobium content as claimed in claim 2, wherein in the third step, the alloy is subjected to one-time vacuum consumable arc smelting, the smelting current is 1.5-10KA, the smelting voltage is 26-36V, and the smelting specification is phi 150-phi 440 mm.
6. The method for smelting the titanium alloy material with the high niobium content as claimed in claim 2, wherein in the step four, the alloy is smelted in a secondary shell type furnace, the smelting current is 9.5-40KA, the smelting voltage is 32-48V, and the smelting specification is phi 220-phi 440 mm.
7. The method for smelting the titanium alloy material with the high niobium content as claimed in claim 2, wherein in the step five, the alloy is smelted by three times of vacuum consumable arc melting, the smelting current is 8.0-25KA, the smelting voltage is 33-38V, and the smelting specification is phi 220-phi 620 mm.
8. The method for smelting the titanium alloy material with the high niobium content as claimed in claim 2, wherein: in the third step, the fourth step and the fifth step, the vacuum degree in the furnace is less than 6.77Pa during smelting.
9. The method for smelting the titanium alloy material with the high niobium content as claimed in claim 2, wherein: the sequence of step four and step five can be changed.
10. The method for smelting the titanium alloy material with the high niobium content as claimed in claim 2, wherein the alloy finished ingot obtained in the fifth step needs to be put into a resistance furnace for homogenization annealing, and the homogenization annealing temperature is 800-.
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Cited By (3)
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| CN113278812A (en) * | 2021-05-21 | 2021-08-20 | 东莞市诺德金属科技有限公司 | Vacuum consumable melting method for high-Mo-content Ti-Mo alloy homogeneous ingot |
| CN114672676A (en) * | 2022-04-02 | 2022-06-28 | 西部钛业有限责任公司 | Preparation method of R60705 zirconium alloy ingot |
| CN116377283A (en) * | 2023-04-14 | 2023-07-04 | 西北有色金属研究院 | Preparation method of titanium-tantalum alloy cast ingot with high tantalum content |
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