Method for preparing high-purity vanadium ingot by electron beam two-step purification and high-purity vanadium ingot
Patent Information
- Application Number
- CN202510595523.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-09
- Publication Date
- 2026-09-18
- Estimated Expiration
- 2045-05-09
AI Technical Summary
[0004]针对上述现有技术中存在的难以规模化生产99.99%以上高纯钒锭的问题,本发明提供了一种电子束两步提纯制备高纯钒铸锭的方法及高纯钒铸锭,可以实现高纯金属钒锭规模化制备,高纯钒铸锭纯度可达99.99%以上
[0023] (1) This invention discloses a method for preparing high-purity vanadium ingots through two-step electron beam purification and the high-purity vanadium ingots. Compared with the traditional vacuum refining method, this invention first removes low-melting-point, high-saturation-vapor-pressure metal impurities such as Al, Fe, and Cr by utilizing the difference in saturated vapor pressure of elements under the action of a low-power electron beam. The density difference between the inclusions and the melt causes inclusions such as Al2O3 and SiO2 to float in the vanadium melt in the water-cooled crucible and be adsorbed by the cold crucible wall during the flow forming process of the ingot. Then, a high-power electron beam is used to rapidly volatilize the vanadium element, and a high-purity vanadium plate is obtained on the collection plate. The high-melting-point, low-saturation-vapor-pressure metal impurities and residual inclusions remain in the water-cooled crucible. The high-purity vanadium ingots finally prepared have a purity of more than 99.99% and a Si content of no more than 0.002%.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of high-purity metal material preparation technology, specifically to a method for preparing high-purity vanadium ingots through a two-step electron beam purification process and the high-purity vanadium ingots themselves. Background Technology
[0002] In recent years, high-purity vanadium (V) has gained increasing attention as an emerging material, becoming an indispensable key functional raw material in applications such as semiconductor devices and nuclear reactors. Vanadium is used to prepare thermistor thin film materials (VOx) for uncooled infrared detectors, and its purity directly affects the core functions of the thermistor thin film, such as resistance uniformity, temperature coefficient of resistance, and noise figure. High-purity vanadium wire is used as the emitter material for self-sufficient detectors in nuclear power plant cores, and its purity directly determines the detector's sensitivity and lifespan. Sputtering targets for semiconductors and functional components in the nuclear industry both require high-purity vanadium ingots with a purity greater than 99.99%.
[0003] The industrial-scale production of high-purity vanadium metal currently mainly employs the active metallothermic reduction method to prepare crude vanadium metal. This crude vanadium metal is then vacuum-melted to obtain the final vanadium product. However, due to the difficulty in removing inclusions such as SiO2 and Al2O3 formed during the metallothermic reduction process, as well as high-melting-point elements like Mo, Nb, and W introduced from the raw materials, during subsequent vacuum melting, the purity is generally between 99% and 99.9%, with Si content typically between 0.03% and 0.05%. This purity does not meet the requirements for advanced semiconductor sputtering targets and functional components in the nuclear industry. In addition, vanadium metal is also produced using molten salt electrolysis and iodination purification methods, but these methods have low yields and are environmentally unfriendly. During molten salt electrolysis, elements such as Al, Cr, and Fe, whose electrode potentials are close to V, cannot be effectively separated through electrolytic purification and are easily contaminated by electrode materials at high temperatures. The high-temperature iodination purification reaction, where V readily reacts with the container, results in higher levels of Fe, Cr, and Mo in the vanadium metal. In addition, the vanadium metal prepared by molten salt electrolysis purification and iodination purification is small in size and cannot be directly processed into further shapes. Summary of the Invention
[0004] To address the problem of difficulty in scaling up the production of high-purity vanadium ingots with a purity of over 99.99% in the existing technologies, this invention provides a method for preparing high-purity vanadium ingots through a two-step electron beam purification process, as well as the high-purity vanadium ingots themselves. This method enables the large-scale production of high-purity metallic vanadium ingots, with a purity of over 99.99% for the high-purity vanadium ingots.
[0005] To achieve the above objectives, the technical solution of the present invention is as follows:
[0006] A method for preparing high-purity vanadium ingots through a two-step electron beam purification process includes the following steps:
[0007] (1) Remove oil and oxides from the surface of vanadium raw materials by physical grinding or chemical cleaning;
[0008] (2) The vanadium raw material processed in step (1) is pushed into the smelting and purification water-cooled crucible in the electron beam smelting furnace. An electron beam with a power of 100-200kW is applied to uniformly scan the vanadium raw material in the smelting and purification water-cooled crucible to remove low melting point and high saturated vapor pressure metal impurities in the vanadium raw material. Some low-density inclusions in the vanadium melt are adsorbed on the wall of the smelting and purification water-cooled crucible. The purified vanadium melt flows into the crystallizer and is smelted by an electron beam with a power of 80-120kW. The electron beam is turned off and the mixture is cooled to obtain the vanadium ingot after the first purification.
[0009] (3) Remove low-melting-point, high-saturation vapor pressure metals adhering to the electron beam melting furnace and inclusions on the walls of water-cooled crucibles used for melting and purification.
[0010] (4) Set up a collecting plate above the water-cooled crucible for smelting and purification, and preheat the collecting plate to 400-600℃;
[0011] (5) The vanadium ingot obtained after the first purification in step (2) is pushed into the water-cooled crucible for smelting and purification in the electron beam smelting furnace. An electron beam with a power of 300-400kW is applied to uniformly scan the vanadium ingot in the water-cooled crucible for smelting and purification. The vanadium element volatilizes and condenses on the collection plate to form a vanadium plate. High melting point, low saturated vapor pressure metal impurities and residual inclusions remain in the water-cooled crucible for smelting and purification.
[0012] (6) Separate the vanadium plate obtained in step (5) from the collection plate, cut it and put it into the crystallizer, apply an electron beam with a power of 80-120kW for melting, turn off the electron beam and cool it to obtain a high-purity vanadium ingot.
[0013] Furthermore, in step (1), the purity of the vanadium raw material is 99.5-99.9%.
[0014] Furthermore, in step (2), the low-melting-point, high-saturated vapor pressure metal includes Al, Fe, and Cr; the inclusions include Al2O3 and SiO2; and the vanadium ingot after the first purification is in the shape of a round rod.
[0015] Furthermore, in steps (2) and (5), the vacuum degree inside the electron beam melting furnace is less than 5 × 10⁻⁶. -3 Pa.
[0016] Furthermore, in step (4), the collecting plate is set 400-700mm above the water-cooled crucible for smelting and purification; the collecting plate is equipped with a thermal resistor; the material of the collecting plate is vanadium and the thickness is 2-5mm.
[0017] Furthermore, in step (5), the high melting point and low saturated vapor pressure metal includes Mo, Nb, and W; the smelting time is 1-4 hours; and the thickness of the vanadium plate is 0.5-3 mm.
[0018] Furthermore, in step (6), the diameter of the high-purity vanadium ingot is 100-200 mm.
[0019] This invention also includes the following technical solutions:
[0020] A high-purity vanadium ingot prepared by the above method.
[0021] Furthermore, its chemical composition by weight percentage includes: V ≥ 99.99%, Fe ≤ 0.0040%, Si ≤ 0.0020%, Zr ≤ 0.0005%, Al ≤ 0.0010%, Cr ≤ 0.0002%, Mo ≤ 0.0005%, and W ≤ 0.0005%.
[0022] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0023] (1) This invention discloses a method for preparing high-purity vanadium ingots through two-step electron beam purification and the high-purity vanadium ingots. Compared with the traditional vacuum refining method, this invention first removes low-melting-point, high-saturation-vapor-pressure metal impurities such as Al, Fe, and Cr by utilizing the difference in saturated vapor pressure of elements under the action of a low-power electron beam. The density difference between the inclusions and the melt causes inclusions such as Al2O3 and SiO2 to float in the vanadium melt in the water-cooled crucible and be adsorbed by the cold crucible wall during the flow forming process of the ingot. Then, a high-power electron beam is used to rapidly volatilize the vanadium element, and a high-purity vanadium plate is obtained on the collection plate. The high-melting-point, low-saturation-vapor-pressure metal impurities and residual inclusions remain in the water-cooled crucible. The high-purity vanadium ingots finally prepared have a purity of more than 99.99% and a Si content of no more than 0.002%.
[0024] (2) The present invention discloses a method for preparing high-purity vanadium ingots by two-step electron beam purification. It only requires the addition of a collection system to the traditional electron beam cold hearth furnace. The preparation process is simple and easy to implement, so that vanadium can be purified to a high purity by electron beam purification alone. Compared with the preparation of vanadium by molten salt electrolysis and iodination, it has the advantages of being environmentally friendly, fast manufacturing speed and high efficiency, and is suitable for industrial-scale production. Attached Figure Description
[0025] The embodiments of the present invention will be further described below with reference to the accompanying drawings, wherein:
[0026] Figure 1 A schematic diagram of the first electron beam purification is shown;
[0027] Figure 2 A schematic diagram of the second electron beam purification is shown;
[0028] Figure 3 A schematic diagram of high-purity vanadium ingot forming is shown;
[0029] 1-Electron gun, 2-Electron gun, 3-Electron beam melting furnace, 4-Feeding system, 5-Water-cooled crucible for melting and purification, 6-Crystallizer, 7-Collection plate. Detailed Implementation
[0030] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.
[0031] A method for preparing high-purity vanadium ingots through a two-step electron beam purification process includes the following steps:
[0032] (1) Remove oil and oxides from the surface of vanadium raw materials by physical grinding or chemical cleaning;
[0033] (2) Reference Appendix Figure 1 The vanadium raw material processed in step (1) is pushed into the smelting and purification water-cooled crucible 5 in the electron beam melting furnace 3 through the feeding system 4, and the vacuum degree in the electron beam melting furnace 3 is kept less than 5×10. -3 Pa, electron gun 1 applies an electron beam with a power of 100-200kW to uniformly scan the vanadium raw material in the water-cooled crucible 5 for smelting and purification, removing low-melting-point, high-saturation vapor pressure metals from the vanadium raw material. Some low-density inclusions in the vanadium melt are adsorbed on the wall of the water-cooled crucible for smelting and purification. The purified vanadium melt flows into the crystallizer 6, where electron gun 2 applies an electron beam with a power of 80-120kW for smelting. The electron beam is then turned off, and the mixture is cooled to obtain the vanadium ingot after the first purification.
[0034] (3) Remove the low-melting-point, high-saturation vapor pressure metals adhering to the electron beam melting furnace 3 and the inclusions on the wall of the water-cooled crucible 5 for melting and purification.
[0035] (4) Set up a collection plate 7 300-700 mm above the water-cooled crucible 5 for smelting and purification, and preheat the collection plate 7 to 400-600℃;
[0036] (5) Reference Appendix Figure 2 The vanadium ingot obtained after the first purification in step (2) is pushed into the water-cooled crucible 5 of the electron beam melting furnace 3 through the feeding system 4, and the vacuum degree in the electron beam melting furnace 3 is kept less than 5×10. -3Pa, electron gun 1 applies an electron beam with a power of 300-400kW to uniformly scan the vanadium ingot in the water-cooled crucible 5 for smelting and purification. The smelting time is 1-4h. The vanadium element volatilizes and condenses on the collection plate 7 to form a vanadium plate with a thickness of 0.5-3mm. High melting point, low saturated vapor pressure metal impurities and residual inclusions remain in the water-cooled crucible 5 for smelting and purification.
[0037] (6) Reference Appendix Figure 3 The vanadium plate obtained in step (5) is separated from the collecting plate 7, cut, and then fed into the crystallizer 6 through the feeding system 4, while maintaining the vacuum degree in the electron beam melting furnace 3 at less than 5 × 10⁻⁶. -3 Pa, an electron beam with a power of 80-120kW is applied to the electron gun 2 for melting, the electron beam is turned off, and the mixture is cooled to obtain a high-purity vanadium ingot.
[0038] The purity of vanadium ingots prepared using the above method was analyzed.
[0039] Example 1
[0040] A method for preparing high-purity vanadium ingots through a two-step electron beam purification process includes the following steps:
[0041] (1) The oil and oxides on the surface of the vanadium raw material are removed by physical grinding or chemical cleaning. The chemical composition of the vanadium raw material by weight percentage includes: V 99.5%, Fe 0.0420%, Si 0.0630%, Zr 0.0005%, Al 0.0220%, Cr 0.0022%, Mo 0.0072%, W 0.0010%;
[0042] (2) The vanadium raw material processed in step (1) is fed into the water-cooled crucible 5 for smelting and purification in the electron beam melting furnace 3 through the feeding system 4, maintaining the vacuum degree in the electron beam melting furnace 3 at less than 5 × 10⁻⁶. -3 Pa, electron gun 1 applies an electron beam with a power of 100kW to uniformly scan the vanadium raw material in the water-cooled crucible 5 for smelting and purification, removing low-melting-point, high-saturation vapor pressure metals from the vanadium raw material. Some low-density inclusions in the vanadium melt are adsorbed on the wall of the water-cooled crucible for smelting and purification. The purified vanadium melt flows into the crystallizer 6, where electron gun 2 applies an electron beam with a power of 120kW for smelting. The electron beam is then turned off and the mixture is cooled to obtain the first purified vanadium ingot.
[0043] (3) Remove the low-melting-point, high-saturation vapor pressure metals adhering to the electron beam melting furnace 3 and the inclusions on the wall of the water-cooled crucible 5 for melting and purification.
[0044] (4) Set up a collection plate 7 700 mm above the water-cooled crucible 5 for smelting and purification, and preheat the collection plate 7 to 600°C.
[0045] (5) The vanadium ingot obtained after the first purification in step (2) is pushed into the water-cooled crucible 5 for smelting and purification in the electron beam melting furnace 3 through the feeding system 4, and the vacuum degree in the electron beam melting furnace 3 is kept less than 5×10. -3 Pa, electron gun 1 applies an electron beam with a power of 400kW to uniformly scan the vanadium ingot in the water-cooled crucible 5 for smelting and purification. The smelting time is 1h. The vanadium element volatilizes and condenses on the collection plate 7 to form a vanadium plate with a thickness of 0.5mm. High melting point, low saturated vapor pressure metal impurities and residual inclusions remain in the water-cooled crucible 5 for smelting and purification.
[0046] (6) Reference Appendix Figure 3 The vanadium plate obtained in step (5) is separated from the collecting plate 7, cut, and then fed into the crystallizer 6 through the feeding system 4, while maintaining the vacuum degree in the electron beam melting furnace 3 at less than 5 × 10⁻⁶. -3 Pa, an electron beam with a power of 80kW is applied to the electron gun 2 for melting, the electron beam is turned off, and the mixture is cooled to obtain a high-purity vanadium ingot.
[0047] The high-purity vanadium ingots prepared, after testing and analysis, have the following chemical composition by weight percentage: V≥99.99%, Fe 0.0036%, Si 0.0017%, Zr 0.0004%, Al 0.0005%, Cr 0.0001%, Mo 0.0002%, W 0.0002%.
[0048] Example 2
[0049] A method for preparing high-purity vanadium ingots through a two-step electron beam purification process includes the following steps:
[0050] (1) The oil and oxides on the surface of the vanadium raw material are removed by physical grinding or chemical cleaning. The chemical composition of the vanadium raw material by weight percentage includes: V 99.5%, Fe 0.0420%, Si 0.0630%, Zr 0.0005%, Al 0.0220%, Cr 0.0022%, Mo 0.0072%, W 0.0010%;
[0051] (2) The vanadium raw material processed in step (1) is fed into the water-cooled crucible 5 for smelting and purification in the electron beam melting furnace 3 through the feeding system 4, maintaining the vacuum degree in the electron beam melting furnace 3 at less than 5 × 10⁻⁶. -3 Pa, electron gun 1 applies an electron beam with a power of 200kW to uniformly scan the vanadium raw material in the water-cooled crucible 5 for smelting and purification, removes low-melting-point, high-saturation vapor pressure metals from the vanadium raw material, and some low-density inclusions in the vanadium melt are adsorbed on the wall of the water-cooled crucible for smelting and purification; the purified vanadium melt flows into the crystallizer 6, electron gun 2 applies an electron beam with a power of 80kW for smelting, the electron beam is turned off, and the mixture is cooled to obtain the vanadium ingot after the first purification.
[0052] (3) Remove the low-melting-point, high-saturation vapor pressure metals adhering to the electron beam melting furnace 3 and the inclusions on the wall of the water-cooled crucible 5 for melting and purification.
[0053] (4) Set up a collection plate 7 400 mm above the water-cooled crucible 5 for smelting and purification, and preheat the collection plate 7 to 400°C.
[0054] (5) The vanadium ingot obtained after the first purification in step (2) is pushed into the water-cooled crucible 5 for smelting and purification in the electron beam melting furnace 3 through the feeding system 4, and the vacuum degree in the electron beam melting furnace 3 is kept less than 5×10. -3 Pa, electron gun 1 applies an electron beam with a power of 300kW to uniformly scan the vanadium ingot in the water-cooled crucible 5 for smelting and purification. The smelting time is 4h. The vanadium element volatilizes and condenses on the collection plate 7 to form a vanadium plate with a thickness of 3mm. High melting point, low saturated vapor pressure metal impurities and residual inclusions remain in the water-cooled crucible 5 for smelting and purification.
[0055] (6) Reference Appendix Figure 3 The vanadium plate obtained in step (5) is separated from the collecting plate 7, cut, and then fed into the crystallizer 6 through the feeding system 4, while maintaining the vacuum degree in the electron beam melting furnace 3 at less than 5 × 10⁻⁶. -3 Pa, an electron beam with a power of 120kW is applied to the electron gun 2 for melting, the electron beam is turned off, and the mixture is cooled to obtain a high-purity vanadium ingot.
[0056] The high-purity vanadium ingots prepared, after testing and analysis, have the following chemical composition by weight percentage: V≥99.99%, Fe 0.0028%, Si 0.0015%, Zr 0.0004%, Al 0.0004%, Cr 0.0001%, Mo 0.0002%, W 0.0002%.
[0057] Example 3
[0058] The difference between this embodiment and Embodiment 1 is that the chemical composition of the vanadium raw material by weight percentage includes: V 99.7%, Fe 0.0350%, Si 0.0490%, Zr 0.0004%, Al 0.0180%, Cr 0.0008%, Mo 0.0067%, W 0.009%, and the remaining parameter settings are the same as in Embodiment 1.
[0059] The high-purity vanadium ingots prepared, after testing and analysis, have the following chemical composition by weight percentage: V≥99.99%, Fe 0.0021%, Si 0.0007%, Zr 0.0002%, Al 0.0002%, Cr 0.0001%, Mo 0.0002%, W 0.0001%.
[0060] Example 4
[0061] The difference between this embodiment and Embodiment 1 is that the chemical composition of the vanadium raw material by weight percentage includes: V 99.9%, Fe 0.0021%, Si 0.0320%, Zr 0.0003%, Al 0.0140%, Cr 0.0005%, Mo 0.0078%, W 0.007%, and the remaining parameter settings are the same as in Embodiment 1.
[0062] The high-purity vanadium ingots prepared, after testing and analysis, have the following chemical composition by weight percentage: V≥99.99%, Fe 0.0007%, Si 0.0002%, Zr 0.0003%, Al 0.0001%, Cr 0.0001%, Mo 0.0001%, W 0.0001%.
[0063] Example 5
[0064] The difference between this embodiment and embodiment 1 is that the refining time in step (5) is 3 hours and the thickness of the collected vanadium plate is 2.2 mm.
[0065] The high-purity vanadium ingots obtained were tested and analyzed, and their chemical composition by weight percentage included: V≥99.99%, Fe 0.0035%, Si 0.00015%, Zr 0.0004%, Al 0.0006%, Cr 0.0001%, Mo 0.0002%, and W 0.0001%.
[0066] Comparative Example 1
[0067] The difference between this comparative example and Example 1 is that in step (2), an electron beam with a power of 80kW is applied to the electron gun 1 to uniformly scan the vanadium raw material in the water-cooled crucible 5 for melting and purification. The other parameter settings are the same as in Example 1.
[0068] The high-purity vanadium ingots prepared, after testing and analysis, have the following chemical composition by weight percentage: V≥99.9%, Fe 0.0120%, Si 0.0022%, Zr 0.0006%, Al 0.0026%, Cr 0.0001%, Mo 0.0002%, W 0.0002%.
[0069] Comparative Example 2
[0070] The difference between this comparative example and Example 1 is that only steps (1) and (2) are performed, and subsequent steps are not performed. All other parameter settings are the same as in Example 1.
[0071] The high-purity vanadium ingots prepared, after testing and analysis, have the following chemical composition by weight percentage: V≥99.9%, Fe 0.0078%, Si 0.0260%, Zr 0.0004%, Al 0.0110%, Cr 0.0002%, Mo 0.0078%, W 0.0012%.
[0072] Comparative Example 3
[0073] The difference between this comparative example and Example 1 is that the preheating temperature of the collection plate 7 in step (4) is 200°C, and the other parameter settings are the same as those in Example 1.
[0074] The vanadium plate collected in step (4) of this comparative example was only 0.3 mm thick and showed signs of peeling and flaking. The amount collected was too small to proceed to the next step of electron beam melting.
[0075] Comparative Example 4
[0076] The difference between this comparative example and Example 1 is that the preheating temperature of the collection plate 7 in step (4) is 700°C, and the other parameter settings are the same as those in Example 1.
[0077] The vanadium plate collected in step (4) of this comparative example was 0.6 mm thick, but it was firmly bonded to the collection plate and not easy to separate, so it was not used for the next step of electron beam melting.
[0078] This invention discloses a two-step electron beam purification method for preparing high-purity vanadium ingots and the high-purity vanadium ingots. Compared with the traditional vacuum refining method, the method first removes low-melting-point, high-saturation-vapor-pressure elements such as Al, Fe, and Cr by utilizing the difference in saturated vapor pressure of elements under the action of a low-power electron beam. Then, it separates inclusions such as Al2O3 and SiO2 in a water-cooled crucible by utilizing the density difference between inclusions and the melt. Afterward, a high-power electron beam is used to rapidly volatilize vanadium, and a high-purity vanadium plate is obtained on the collection plate. High-melting-point, low-saturation-vapor-pressure metal impurities and residual inclusions remain in the water-cooled crucible. The final high-purity vanadium ingot has a purity of over 99.99% and a Si content of no more than 0.002%.
[0079] The present invention discloses a two-step electron beam purification method for preparing high-purity vanadium ingots. It only requires the addition of a collection system to a traditional electron beam cold hearth furnace. The preparation process is simple and easy to implement, and vanadium can be purified to a high purity by electron beam purification alone. Compared with the purification of vanadium by molten salt electrolysis and iodination, it has the advantages of being environmentally friendly, fast in manufacturing, and efficient, and is suitable for industrial-scale production.
[0080] The foregoing descriptions have outlined some exemplary embodiments of the present invention. It is understood that these embodiments are merely illustrative and do not constitute a limitation on the scope of protection of the present invention. Features in these embodiments can be rearranged in suitable ways, and the resulting solutions remain within the scope of protection claimed by the present invention. All other embodiments obtained by those skilled in the art based on the foregoing embodiments without inventive effort, i.e., all modifications, equivalent substitutions, and improvements made within the spirit and principles of this application, fall within the scope of protection claimed by the present invention.
Claims
1. A method for preparing high-purity vanadium ingots through a two-step electron beam purification process, characterized in that, Includes the following steps: (1) Remove oil and oxides from the surface of vanadium raw materials by physical grinding or chemical cleaning; (2) The vanadium raw material processed in step (1) is pushed into the smelting and purification water-cooled crucible in the electron beam smelting furnace. An electron beam with a power of 100-200kW is applied to uniformly scan the vanadium raw material in the smelting and purification water-cooled crucible to remove low melting point and high saturated vapor pressure metal impurities in the vanadium raw material. Some low-density inclusions in the vanadium melt are adsorbed on the wall of the smelting and purification water-cooled crucible. The purified vanadium melt flows into the crystallizer and is smelted by an electron beam with a power of 80-120kW. The electron beam is turned off and the mixture is cooled to obtain the vanadium ingot after the first purification. (3) Remove low-melting-point, high-saturation vapor pressure metals adhering to the electron beam melting furnace and inclusions on the walls of water-cooled crucibles used for melting and purification. (4) Set up a collecting plate above the water-cooled crucible for smelting and purification, and preheat the collecting plate to 400-600℃; (5) The first purified vanadium ingot obtained in step (2) is pushed into the smelting and purification water-cooled crucible in the electron beam smelting furnace. An electron beam with a power of 300-400kW is applied to uniformly scan the vanadium ingot in the smelting and purification water-cooled crucible. The vanadium element volatilizes and condenses on the collection plate to form a vanadium plate. High melting point, low saturated vapor pressure metal impurities and residual inclusions remain in the smelting and purification water-cooled crucible. (6) Separate the vanadium plate obtained in step (5) from the collection plate, cut it and put it into the crystallizer, apply an electron beam with a power of 80-120kW for melting, turn off the electron beam and cool it to obtain a high-purity vanadium ingot.
2. The method for preparing high-purity vanadium ingots through a two-step electron beam purification process according to claim 1, characterized in that, In step (1), the purity of the vanadium raw material is 99.5-99.9%.
3. The method for preparing high-purity vanadium ingots through a two-step electron beam purification process according to claim 1, characterized in that, In step (2), the low-melting-point, high-saturated vapor pressure metal includes Al, Fe, and Cr; the inclusions include Al2O3 and SiO2; and the vanadium ingot after the first purification is in the shape of a round rod.
4. The method for preparing high-purity vanadium ingots through a two-step electron beam purification process according to claim 1, characterized in that, In steps (2) and (5), the vacuum degree in the electron beam melting furnace is less than 5 x 10 -3 Pa.
5. The method for preparing high-purity vanadium ingots through a two-step electron beam purification process according to claim 1, characterized in that, In step (4), the collecting plate is set 400-700mm above the water-cooled crucible for smelting and purification; the collecting plate is equipped with a thermal resistor; the collecting plate is made of vanadium and has a thickness of 2-5mm.
6. The method for preparing high-purity vanadium ingots through a two-step electron beam purification process according to claim 1, characterized in that, In step (5), the high melting point and low saturated vapor pressure metals include Mo, Nb, and W; the smelting time is 1-4 hours; and the thickness of the vanadium plate is 0.5-3 mm.
7. The method for preparing high-purity vanadium ingots through a two-step electron beam purification process according to claim 1, characterized in that, In step (6), the diameter of the high-purity vanadium ingot is 100-200 mm.
Citation Information
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