Preparation method of low-oxygen titanium-containing powder

Abstract

The invention belongs to the technical field of thermometallurgy, and particularly relates to a preparation method of low-oxygen titanium-containing powder. The method comprises the following steps: deoxidizing titanium-containing powder and metal lithium in hydrogen or mixed gas of hydrogen and protective gas to obtain a deoxidized material; the titanium-containing powder comprises titanium powder and / or titanium alloy powder; the deoxidation temperature is 300 to 600 DEG C; carrying out vacuum distillation on the deoxidized material to obtain low-oxygen titanium-containing powder and recycled metal lithium; the temperature of the vacuum distillation is 400 to 600 DEG C; the oxygen content of the low-oxygen titanium-containing powder is smaller than 1500 ppm. The oxygen content of the low-oxygen titaniferous powder prepared through the method is lower than 1500 ppm, the low-oxygen titaniferous powder is not sticky, particles are complete, the mechanical property of the low-oxygen titaniferous powder cannot be damaged, and impurities are not introduced to pollute titanium or titanium alloy.

Description

Technical Field

[0001] The invention belongs to the technical field of pyrometallurgy, and in particular relates to a method for preparing low-oxygen titanium-containing powder. Background Art

[0002] With the development of science and technology, people's demand for special metal materials has become stronger. Titanium and titanium alloys are favored in the fields of military industry, aerospace, marine engineering and chemical industry due to their excellent performance. However, the extremely low utilization rate makes titanium or titanium alloy products expensive and cannot be used on a large scale in the civilian field, which seriously restricts the development of the titanium industry.

[0003] With the maturity of 3D printing technology and powder metallurgy technology, a solution has been found for the low utilization rate of titanium and titanium alloy materials. Unfortunately, titanium is very easy to combine with oxygen to form titanium oxide alloys, and too high an oxygen content will seriously affect the value of titanium or titanium alloys. In the process of preparing titanium or titanium alloy powders, the oxygen content of titanium or titanium alloy powders will increase rapidly, usually reaching 5000 to 15000 ppm. Titanium parts prepared using this kind of titanium or titanium alloy powder cannot meet the needs of production and life because of the excessively high oxygen content, which will lead to a decrease in ductility, strength and corrosion resistance of titanium parts.

[0004] With the huge application prospects of titanium powder, many scientists have developed a variety of deoxidation methods, among which calcium vapor deoxidation, molten salt-assisted alkali metal thermochemical deoxidation, molten salt-assisted rare earth and rare earth chloride deoxidation are the most common. However, these methods have many fatal shortcomings, such as the deoxidation temperature is too high, resulting in the damage of the mechanical properties of titanium or titanium alloy powder, and the titanium or titanium alloy powder is contaminated by deoxidizer or molten salt. Summary of the invention

[0005] In view of this, the object of the present invention is to provide a method for preparing low-oxygen titanium-containing powder. The oxygen content of the low-oxygen titanium-containing powder prepared by this method is lower than 1500ppm, and the low-oxygen titanium-containing powder does not stick together, the particles are intact, its mechanical properties will not be destroyed, and impurities will not be introduced to contaminate titanium or titanium alloys.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] The present invention provides a method for preparing a low-oxygen titanium-containing powder, comprising the following steps:

[0008] Deoxidizing titanium-containing powder and metallic lithium in hydrogen or a mixed gas of hydrogen and protective gas to obtain a deoxidized material; the titanium-containing powder includes titanium powder and / or titanium alloy powder; the deoxidation temperature is 300-600°C;

[0009] The deoxidized material is subjected to vacuum distillation to obtain low-oxygen titanium-containing powder and recover metallic lithium; the temperature of the vacuum distillation is 400-600° C.; the oxygen content of the low-oxygen titanium-containing powder is less than 1500 ppm.

[0010] Preferably, the mass ratio of the titanium-containing powder to metallic lithium is 5 to 10:1.

[0011] Preferably, the deoxidation insulation time is 8 to 32 hours.

[0012] Preferably, the insulation time of the vacuum distillation is 6 to 12 hours.

[0013] Preferably, the heating rate to the deoxidation temperature is 3-7°C / min.

[0014] Preferably, the shielding gas is argon; and the mass concentration of hydrogen in the mixed gas of hydrogen and shielding gas is ≥1% and <100%.

[0015] Preferably, the vacuum degree of the vacuum distillation is ≤50Pa.

[0016] Preferably, after the vacuum distillation, the method further comprises: washing and drying the solid obtained by the vacuum distillation in a protective atmosphere in sequence to obtain the low-oxygen titanium-containing powder; and recovering the gas generated by the vacuum distillation by vacuuming to obtain the recovered metallic lithium.

[0017] Preferably, the protective atmosphere is argon.

[0018] Preferably, the vacuum is evacuated to below 50 Pa.

[0019] The present invention provides a method for preparing a low-oxygen titanium-containing powder, comprising the following steps: deoxidizing a titanium-containing powder and metal lithium in hydrogen or a mixed gas of hydrogen and protective gas to obtain a deoxidized material; the titanium-containing powder includes titanium powder and / or titanium alloy powder; the deoxidation temperature is 300-600°C; vacuum distilling the deoxidized material to obtain a low-oxygen titanium-containing powder and recover metal lithium; the vacuum distillation temperature is 400-600°C; the oxygen content of the low-oxygen titanium-containing powder is less than 1500ppm. The present invention utilizes metal lithium and hydrogen to deoxidize a titanium-containing powder (titanium powder and / or titanium alloy powder), hydrogen reduces the stability of a Ti-O solid solution, thereby achieving thermochemical deoxidation of metal lithium, and a low deoxidation temperature can prevent the titanium-containing powder from sintering or damaging the mechanical properties and morphology of the titanium-containing powder, and then removing lithium by vacuum distillation, and dissolved hydrogen is also removed from titanium and titanium alloys during the vacuum distillation process. The present invention can effectively reduce the oxygen content of titanium or titanium alloy to below 1500ppm, and does not introduce deoxidizers such as hydrogen and impurities such as Li to pollute titanium or titanium alloy. In addition, the prepared low-oxygen titanium-containing powder is non-adhesive and has complete particles, and is suitable for powder metallurgy and 3D printing.

[0020] In this method, the deoxidation temperature is low, the titanium or titanium alloy powder is clean, the deoxidation process is easy to operate, the process is simple, no toxic and harmful substances are generated, the required equipment is simple, the production cost is low, it has great economic and environmental benefits, and realizes the production of low-oxygen titanium powder and titanium alloy powder in the industrial field. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 Schematic diagram of the preparation process of low-oxygen titanium-containing powder in an embodiment of the present invention;

[0022] Figure 2 This is a physical picture of the low-oxygen titanium powder prepared in Example 1. DETAILED DESCRIPTION

[0023] The present invention provides a method for preparing a low-oxygen titanium-containing powder, comprising the following steps:

[0024] Deoxidizing titanium-containing powder and metallic lithium in hydrogen or a mixed gas of hydrogen and protective gas to obtain a deoxidized material; the titanium-containing powder includes titanium powder and / or titanium alloy powder; the deoxidation temperature is 300-600°C;

[0025] The deoxidized material is subjected to vacuum distillation to obtain low-oxygen titanium-containing powder and recover metallic lithium; the temperature of the vacuum distillation is 400-600° C.; the oxygen content of the low-oxygen titanium-containing powder is less than 1500 ppm.

[0026] Unless otherwise specified, the present invention has no special requirements on the sources of the raw materials used, and commercially available products known to those skilled in the art may be used.

[0027] The present invention deoxidizes titanium-containing powder and metallic lithium in hydrogen or a mixed gas of hydrogen and protective gas to obtain deoxidized material.

[0028] As an embodiment, the titanium-containing powder includes titanium powder and / or titanium alloy powder, and in a specific embodiment, it is titanium powder or titanium alloy powder; the mass ratio of the titanium-containing powder to metallic lithium is 5 to 10:1, and in a specific embodiment, it is 5 to 7:1.

[0029] The deoxidation temperature of the prior art is above 800°C, because the melting point of metallic lithium is low, while other metals have high melting points, and the deoxidation temperature needs to reach above the melting point of the deoxidizer. Since other types of deoxidizers have high melting points, they will cause sintering or contamination of titanium or titanium alloy powders, and potassium deoxidation effect is poor. At the deoxidation temperature provided by the present invention, only metallic lithium has the best deoxidation effect. As the amount of metallic lithium increases, the deoxidation effect will increase, but it will not be greatly improved. However, metallic lithium is expensive. Within the amount range of metallic lithium provided by the present invention, the deoxidation effect can meet the requirements.

[0030] As an embodiment, the particle size of the titanium-containing powder is ≤120μm, and in a specific embodiment, it is 40-50μm; the oxygen content of the titanium-containing powder is 4500-5500ppm, and in a specific embodiment, it is 4650-5020ppm; the particle size of the metallic lithium is 1-5mm, and in a specific embodiment, it is 3-4mm.

[0031] As an embodiment, the protective gas is argon; the mass concentration of hydrogen in the mixed gas of hydrogen and protective gas is ≥1% and <100%, and in a specific embodiment, it is 10-20%; the hydrogen or the mixed gas of hydrogen and protective gas is introduced from the bottom of the titanium-containing powder and metallic lithium. The present invention does not specifically limit the flow rate of hydrogen or the mixed gas of hydrogen and protective gas, and the gas can be introduced at a relatively low flow rate to prevent the titanium-containing powder and metallic lithium from being blown away. Since the inner diameter of the bottom vent hole of the titanium crucible is 5 mm, there will not be a large flow rate at a relatively low gas flow rate.

[0032] The present invention introduces hydrogen or a mixed gas of hydrogen and protective gas from the bottom, which not only ensures that H2 can fully react with titanium powder or titanium alloy powder, but also helps to stir the deoxidation process and promote the deoxidation reaction.

[0033] Hydrogen can reduce the stability of titanium oxide solid solution. As the amount of hydrogen increases, the deoxidation effect increases, but when the mass concentration of hydrogen in the mixed gas exceeds 10%, the increase is no longer obvious.

[0034] As an implementation mode, the deoxidation temperature is 300-600° C., and in a specific embodiment, it is 400-600° C.; the deoxidation insulation time is 8-32 hours, and in a specific embodiment, it is 12-16 hours.

[0035] Under the same deoxygenation time, within the range set by the present invention, the deoxygenation effect is improved as the deoxygenation temperature is increased; under the same deoxygenation temperature, the deoxygenation effect is improved as the deoxygenation time is prolonged. After the deoxygenation time reaches 16 hours, the deoxygenation effect is not significantly improved by prolonging the time. The deoxygenation time range provided by the present invention can ensure thorough deoxygenation.

[0036] As an implementation manner, the heating rate to the deoxidation temperature is 3 to 7°C / min, and in a specific embodiment is 4 to 5°C / min.

[0037] As an implementation mode, the deoxidation equipment is a titanium crucible with a vent hole at the bottom and a heating furnace, the vent hole at the bottom of the titanium crucible is connected to the vent pipe of the heating furnace; the inner diameter of the vent hole is 5 mm.

[0038] As an implementation manner, before deoxidation, it further includes: introducing hydrogen or a mixed gas of hydrogen and a protective gas into the furnace cavity of the heating furnace until only hydrogen or a mixed gas of hydrogen and a protective gas remains in the furnace cavity, and then turning on the heating furnace for heating. In the present invention, the feeding amounts of hydrogen and argon are controlled by the ventilation valves installed in front of the high-precision gas mass flow controllers in cooperation with the valves of the gas cylinders.

[0039] As an implementation manner, after the deoxidation, it further includes: closing the feeding of hydrogen, cooling the deoxidized product to room temperature in argon, taking out the titanium crucible, and blocking the ventilation holes at the bottom of the titanium crucible; the cooling process is natural cooling.

[0040] The main reaction during the deoxidation process is Ti[O] x +Li+H2→Li2O+Ti[O] y [H] z (y < x), H2 reduces the stability of the Ti-O solid solution, thereby realizing the thermochemical deoxidation of metallic lithium.

[0041] After obtaining the deoxidized material, the present invention performs vacuum distillation on the deoxidized material to obtain low-oxygen titanium-containing powder and recovered metallic lithium.

[0042] As an implementation manner, the temperature of the vacuum distillation is 400 - 600 °C, and in specific embodiments, it is 450 - 550 °C; the heat preservation time of the vacuum distillation is 6 - 12 h, and in specific embodiments, it is 8 - 10 h.

[0043] The temperature of the vacuum distillation provided by the present invention below the sintering temperature of titanium powder (above 900 °C) can prevent the deoxidized material from sintering or damaging the mechanical properties and morphology of the deoxidized material. Too high a temperature will cause cracking of the deoxidized material, thereby damaging its mechanical properties or shape. The vacuum distillation should ensure that the metallic lithium volatilizes completely. The time of the vacuum distillation is affected by the particle size of the deoxidized material. The smaller the particle size, the longer the distillation time. During the process of removing lithium by vacuum distillation, it can also promote the removal of dissolved hydrogen from titanium or titanium alloy.

[0044] As an implementation manner, the vacuum degree of the vacuum distillation is ≤ 50 Pa, and in specific embodiments, it is 5 - 30 Pa.

[0045] As an implementation manner, the equipment used for the vacuum distillation is a vacuum furnace; before performing the vacuum distillation, the present invention further includes: cleaning the vacuum furnace with argon.

[0046] As an embodiment, after the vacuum distillation, the method further comprises: washing and drying the vacuum distilled solid in a protective atmosphere in sequence to obtain the low-oxygen titanium-containing powder; recovering the gas generated by the vacuum distillation by vacuuming to obtain the recovered metallic lithium; reusing the recovered metallic lithium in the deoxidation process; and vacuuming to below 50 Pa, 4 to 10 Pa in a specific embodiment. Increasing the vacuum degree can increase the volatilization rate of metallic lithium.

[0047] As an implementation mode, the protective atmosphere is argon; the reagent used for the water washing is oxygen-free deionized water; the number of water washings is ≥3 times, and in the specific embodiment, it is 3 to 5 times; the water washing is an immersion method water washing, specifically: after adding oxygen-free deionized water to the solid after vacuum distillation, it is continuously stirred; the drying temperature is 50 to 70°C, and in the specific embodiment, it is 50 to 60°C. The present invention does not specifically limit the drying time until it is completely dried. Boiling can remove the gas (mainly oxygen and nitrogen) dissolved in the deionized water to obtain oxygen-free deionized water. Washing and drying in a protective atmosphere can prevent the gas (mainly oxygen and nitrogen) from contaminating the low-oxygen titanium-containing powder after vacuum distillation.

[0048] As an embodiment, the present invention also includes: recycling the waste liquid generated by the water washing for multiple times, and then chlorinating and concentrating the waste liquid, electrolyzing the obtained lithium chloride to produce metallic lithium and chlorine, and the metallic lithium is reused in the deoxidation process, and the hydrogen chloride gas generated by the reaction of the chlorine and hydrogen is reused in the chlorination and concentration process; the multiple times are 4 to 7 times, and 5 to 6 times in the specific embodiment; the water washing is washing with oxygen-free pure water; the chlorination and concentration is first concentrated by natural airing, and the lithium hydroxide concentrated liquid obtained by concentration is chlorinated with hydrogen chloride gas to obtain lithium chloride. The present invention recycles the waste liquid generated by the water washing for multiple times for water washing, and can also increase the concentration of lithium ions in the waste liquid. In order to save energy, natural airing and concentration are used, and the concentrated lithium hydroxide is chlorinated with hydrogen chloride gas to obtain lithium chloride. The lithium chloride is electrolyzed to produce lithium and chlorine, and the chlorine and hydrogen react to prepare the hydrogen chloride gas used for chlorination. The high-value metallic lithium can be recycled, reducing production costs.

[0049] Figure 1The figure is a schematic diagram of the preparation process of low-oxygen titanium-containing powder in an embodiment of the present invention. The present invention is carried out by deoxidizing titanium or titanium alloy powder and metallic lithium in a mixed gas of hydrogen and protective gas, vacuum distilling the obtained deoxidation product, recovering the metallic lithium for reuse in the deoxidation process, washing the obtained titanium or titanium alloy powder with water, and concentrating the generated waste liquid by chlorination. The obtained lithium chloride is electrolyzed to generate metallic lithium that is further reused in the deoxidation process. Compared with the existing methods, the present invention utilizes low-temperature deoxidation to obtain the optimal mechanical properties of low-oxygen titanium-containing powder (titanium or titanium alloy powder), saves energy consumption, does not use acid and alkali solution, recycles metallic lithium, reduces costs and increases efficiency, does not generate the three wastes, and is conducive to sustainable development. The equipment used in this method is simple to manufacture and operate, and the obtained titanium or titanium alloy powder has a low oxygen content and does not introduce impurities.

[0050] As an embodiment, the low-oxygen titanium-containing powder comprises deoxidized titanium powder and / or titanium alloy powder; the oxygen content of the low-oxygen titanium-containing powder is less than 1500 ppm, and in a specific embodiment, it is 960 to 1480 ppm.

[0051] The present invention can effectively reduce the oxygen content of titanium or titanium alloy to below 1500ppm, and does not introduce deoxidizers such as hydrogen and impurities such as Li to pollute titanium or titanium alloy. In addition, the prepared low-oxygen titanium-containing powder is non-adhesive and has complete particles, and is suitable for powder metallurgy and 3D printing.

[0052] The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, but they should not be construed as limiting the protection scope of the present invention.

[0053] Example 1

[0054] 300 g of titanium powder (oxygen content of 4650 ppm, particle size of 40-50 μm) and 60 g of metallic lithium (particle size of 3-4 mm) were mixed and added to a titanium crucible with a vent hole at the bottom (inner diameter of 5 mm), the mass ratio of titanium powder to metallic lithium being 5:1, the vent hole at the bottom of the titanium crucible being connected to the vent pipe of the heating furnace, the vent valve installed in front of the high-precision gas mass flow controller was opened to introduce a mixed gas of hydrogen and argon from the bottom of the titanium powder and metallic lithium, wherein the mass concentration of hydrogen was 10%, until there was only a mixed gas of hydrogen and argon in the furnace chamber of the heating furnace, then the heating furnace was turned on for heating, the heating rate was set to 4°C / min, the deoxidation temperatures were set to 400°C, 450°C, 500°C, 550°C, 600°C, respectively, and the temperature was kept at 400°C, 450°C, 500°C, 550°C, 600°C ...600°C. The temperature is kept at 32 hours for deoxidation. After the heat preservation is completed, the hydrogen is turned off and argon is continued to be introduced. After the heating furnace is cooled to room temperature, the titanium crucible is taken out to block the air hole at the bottom thereof, and vacuum distillation is performed in a vacuum furnace after argon cleaning. The distillation temperature is set to 500°C, the vacuum degree is 5Pa, and the vacuum distillation time is 12 hours. After the vacuum distillation is completed, the vacuum is evacuated to 10Pa to recover the metallic lithium, and the recovered metallic lithium is reused in the deoxidation process. After the vacuum distillation, the solid is washed with oxygen-free deionized water in the argon chamber for 5 times to remove residual impurities, and the water washing is an immersion method water washing, specifically: after adding oxygen-free deionized water to the solid after vacuum distillation, it is continuously stirred, and dried at 50°C in a high-purity argon atmosphere until it is completely dry to obtain low-oxygen titanium powder;

[0055] After recycling the waste liquid generated by the water washing for 5 times, it is washed with oxygen-free pure water and then concentrated by natural airing. The lithium hydroxide concentrated liquid obtained by concentration is chlorinated with hydrogen chloride gas, and the obtained lithium chloride is electrolyzed to produce metallic lithium and chlorine. The metallic lithium is reused in the deoxygenation process, and the hydrogen chloride gas generated by the reaction of chlorine and hydrogen is reused in the chlorination concentration process.

[0056] The results of the low-oxygen titanium powder finally obtained in this example are shown in Table 1.

[0057] Table 1 Oxygen content analysis of low oxygen titanium powder

[0058]

[0059] Example 2

[0060] 300 g of titanium powder (oxygen content of 5020 ppm, particle size of 40-50 μm) and 60 g of metallic lithium (particle size of 3-4 mm) were mixed and added to a titanium crucible with a vent hole at the bottom (inner diameter of 5 mm), the mass ratio of titanium powder to metallic lithium being 5:1, the vent hole at the bottom of the titanium crucible being connected to the vent pipe of the heating furnace, the vent valve installed in front of the high-precision gas mass flow controller was opened to introduce a mixed gas of hydrogen and argon from the bottom of the titanium powder and metallic lithium, wherein the mass concentration of hydrogen was 10%, until there was only a mixed gas of hydrogen and argon in the furnace chamber of the heating furnace, then the heating furnace was turned on for heating, the heating rate was set to 4°C / min, the deoxidation temperature was set to 600°C, and the insulation time was 4h, 8h, 12h, 16h, 2h, respectively. 4h, 32h, deoxidation, after the insulation is completed, turn off the introduction of hydrogen, continue to introduce argon, after the heating furnace is cooled to room temperature, take out the titanium crucible and block the vent at the bottom, and perform vacuum distillation in a vacuum furnace after argon cleaning. The distillation temperature is set to 500°C, the vacuum degree is 5Pa, and the vacuum distillation time is 12h. After the vacuum distillation is completed, evacuate to 10Pa to recover metallic lithium, and the recovered metallic lithium is reused in the deoxidation process. After the vacuum distillation, the solid is washed with oxygen-free deionized water in the argon chamber for 5 times to remove residual impurities, and the water washing is an immersion water washing, specifically: after adding oxygen-free deionized water to the solid after vacuum distillation, it is continuously stirred, and dried at 50°C in a high-purity argon atmosphere until it is completely dry to obtain low-oxygen titanium powder;

[0061] The waste liquid generated by the water washing is recycled for 5 times, washed with oxygen-free pure water, and then concentrated by natural airing. The lithium hydroxide concentrated liquid obtained by concentration is chlorinated with hydrogen chloride gas, and the obtained lithium chloride is electrolyzed to produce metallic lithium and chlorine. The metallic lithium is reused in the deoxygenation process, and the hydrogen chloride gas generated by the reaction of chlorine and hydrogen is reused in the chlorination concentration process.

[0062] The results of the low-oxygen titanium powder finally obtained in this example are shown in Table 2.

[0063] Table 2 Oxygen content analysis of low oxygen titanium powder

[0064]

[0065] Example 3

[0066] 300g of titanium alloy powder (TC4, Ti-6Al-4V, oxygen content of 4820ppm) with particle sizes of ≤1μm, 1-10μm, 20-30μm, 40-50μm, 60-80μm, and 100-120μm were selected and mixed with 60g of metallic lithium (particle size of 3-4mm) and added into a titanium crucible with a vent hole at the bottom (inner diameter of 5mm), the mass ratio of TC4 powder to metallic lithium was 5:1, the vent hole at the bottom of the titanium crucible was connected to the vent pipe of the heating furnace, the vent valve installed in front of the high-precision gas mass flow controller was opened to pass a mixed gas of hydrogen and argon from the bottom of the titanium powder and the metallic lithium, wherein the mass concentration of hydrogen was 10%, until there was only a mixed gas of hydrogen and argon in the furnace chamber of the heating furnace, the heating furnace was turned on for heating, and the heating rate was set to 4°C / min, set the deoxidation temperature to 550°C, the insulation time to 12h, deoxidation, after the insulation is completed, turn off the introduction of hydrogen, continue to introduce argon, cool the heating furnace to room temperature, take out the titanium crucible and block the vent at the bottom, and perform vacuum distillation in a vacuum furnace after argon cleaning, the distillation temperature is set to 500°C, the vacuum degree is 5Pa, and the vacuum distillation time is 12h. After the vacuum distillation is completed, evacuate to 10Pa to recover metallic lithium, and the recovered metallic lithium is reused in the deoxidation process, the solid after vacuum distillation is washed with oxygen-free deionized water 5 times in the argon chamber to remove residual impurities, and the water washing is an immersion method water washing, specifically: after adding oxygen-free deionized water to the solid after vacuum distillation, it is continuously stirred, and dried at 50°C in a high-purity argon atmosphere until it is completely dry to obtain a low-oxygen titanium alloy powder;

[0067] The waste liquid generated by the water washing is recycled for 5 times, washed with oxygen-free pure water, and then concentrated by natural airing. The lithium hydroxide concentrated liquid obtained by concentration is chlorinated with hydrogen chloride gas, and the obtained lithium chloride is electrolyzed to produce metallic lithium and chlorine. The metallic lithium is reused in the deoxygenation process, and the hydrogen chloride gas generated by the reaction of chlorine and hydrogen is reused in the chlorination concentration process.

[0068] The results of the low-oxygen titanium alloy powder finally obtained in this example are shown in Table 3.

[0069] Table 3 Oxygen content analysis of low oxygen titanium alloy powder

[0070]

[0071] It can be seen from the above table that the oxygen content of the low-oxygen titanium powder or low-oxygen titanium alloy powder obtained in Examples 1 to 3 is generally 900 to 1500 ppm, the yield of the low-oxygen titanium powder or low-oxygen titanium alloy powder is above 99%, and the metal lithium recovery rate is above 90%.

[0072] Figure 2This is a real picture of the low-oxygen titanium powder prepared in Example 1. As can be seen from the figure, the low-oxygen titanium powder has good particle uniformity, and the low-oxygen titanium powder is observed under a microscope to have a complete spherical shape, and the powders are not adhered to each other. In the present invention, the deoxidation temperature is low, the titanium powder will not sinter, and the titanium powder particles will not deform.

[0073] Although the above embodiment describes the present invention in detail, it is only a part of the embodiments of the present invention rather than all the embodiments. People can also obtain other embodiments based on this embodiment without creativity, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A method for preparing a low-oxygen titanium-containing powder, characterized in that: The following steps are involved: Deoxidizing titanium-containing powder and metallic lithium in hydrogen or a mixed gas of hydrogen and protective gas to obtain a deoxidized material; the titanium-containing powder includes titanium powder and / or titanium alloy powder; the deoxidation temperature is 300-600°C; The deoxidized material is subjected to vacuum distillation to obtain low-oxygen titanium-containing powder and recover metallic lithium; the temperature of the vacuum distillation is 400-600° C.; the oxygen content of the low-oxygen titanium-containing powder is less than 1500 ppm.

2. The preparation method according to claim 1, characterized in that: The mass ratio of the titanium-containing powder to metallic lithium is 5 to 10:

1.

3. The preparation method according to claim 1, characterized in that: The deoxidation insulation time is 8 to 32 hours.

4. The preparation method according to claim 1, characterized in that: The insulation time of the vacuum distillation is 6 to 12 hours.

5. The preparation method according to claim 1 or 3, characterized in that: The heating rate to the deoxidation temperature is 3-7°C / min.

6. The preparation method according to claim 1, characterized in that: The protective gas is argon; the mass concentration of hydrogen in the mixed gas of hydrogen and protective gas is ≥1% and <100%.

7. The preparation method according to claim 1 or 4, characterized in that: The vacuum degree of the vacuum distillation is ≤50Pa.

8. The preparation method according to claim 1, characterized in that: After the vacuum distillation, the method further includes: washing and drying the solid obtained by the vacuum distillation in a protective atmosphere in sequence to obtain the low-oxygen titanium-containing powder; and recovering the gas generated by the vacuum distillation by vacuuming to obtain the recovered metallic lithium.

9. The preparation method according to claim 8, characterized in that: The protective atmosphere is argon.

10. The preparation method according to claim 8, characterized in that: The vacuum is pumped to below 50 Pa.

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