A method for preparing a low-oxygen titanium-containing powder

Abstract

The present application belongs to pyrometallurgical technical field, and particularly relates to a preparation method of low-oxygen titanium-containing powder. The present application carries out deoxidation on titanium-containing powder and metal lithium in hydrogen or mixed gas of hydrogen and protective gas to obtain deoxidized material; the titanium-containing powder comprises titanium powder and / or titanium alloy powder; the deoxidation temperature is 300-600 DEG C; the deoxidized material is subjected to vacuum distillation to obtain low-oxygen titanium-containing powder and recycled metal lithium; the vacuum distillation temperature is 400-600 DEG C; and the oxygen content of the low-oxygen titanium-containing powder is less than 1500 ppm. The oxygen content of the low-oxygen titanium-containing powder prepared by the method is less than 1500 ppm, the low-oxygen titanium-containing powder is not adhered, the particle is complete, the mechanical property is not damaged, and no impurity is introduced to contaminate titanium or titanium alloy.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of pyrometallurgy, and particularly relates to a preparation method of low-oxygen titanium-containing powder. BACKGROUND

[0002] With the development of science and technology, people's demand for special metal materials is increasingly strong. Titanium and titanium alloy are favored in the fields of military industry, aerospace, ocean engineering and chemical industry due to their excellent performance. However, the extremely low utilization rate leads to high prices of titanium or titanium alloy products, which cannot be used on a large scale in civilian fields, and seriously limits the development of the titanium industry.

[0003] With the maturity of 3D printing technology and powder metallurgy technology, a way out has been found for the low utilization rate of titanium and titanium alloy materials. Unfortunately, titanium is extremely easy to combine with oxygen to form titanium-oxygen alloy, and too high oxygen content will seriously affect the value of titanium or titanium alloy. During the preparation of titanium or titanium alloy powder, the oxygen content of the titanium or titanium alloy powder will quickly increase, usually reaching 5000-15000ppm. Titanium parts prepared using such titanium or titanium alloy powder will have decreased ductility, reduced strength and weakened corrosion resistance due to the excessively high oxygen content, which cannot meet the production and life needs.

[0004] Under the huge application prospect of titanium powder, many scientists have developed various deoxidation methods, such as calcium vapor deoxidation, molten salt assisted alkali metal thermochemical deoxidation, and molten salt assisted rare earth and rare earth chloride deoxidation. However, these methods have many fatal defects, such as excessively high deoxidation temperature leading to damage of the mechanical properties of titanium or titanium alloy powder, and contamination of titanium or titanium alloy powder by deoxidizing agent or molten salt. SUMMARY

[0005] Therefore, the purpose of the present application is to provide a preparation method of low-oxygen titanium-containing powder, which has an oxygen content of less than 1500ppm, and the low-oxygen titanium-containing powder is not sticky, the particles are complete, and the mechanical properties are not damaged, and no impurities are introduced to contaminate titanium or titanium alloy.

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

[0007] The present application provides a preparation method of low-oxygen titanium-containing powder, comprising the following steps:

[0008] The titanium-containing powder and metallic lithium are deoxidized in hydrogen or a mixed gas of hydrogen and a protective gas to obtain deoxidized material; the titanium-containing powder comprises titanium powder and / or titanium alloy powder; the deoxidization temperature is 300-600℃;

[0009] The deoxidized material is vacuum distilled to obtain low-oxygen titanium-containing powder and recycled lithium; the temperature of the vacuum distillation is 400-600 DEG C; and the oxygen content of the low-oxygen titanium-containing powder is < 1500 ppm.

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

[0011] Preferably, the holding time for the deoxidization is 8-32 h.

[0012] Preferably, the holding time for the vacuum distillation is 6-12 h.

[0013] Preferably, the heating rate for heating to the deoxidization temperature is 3-7 DEG C / min.

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

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

[0016] Preferably, after the vacuum distillation, the following steps are further included: the solid obtained by the vacuum distillation is sequentially washed with water and dried in a protective gas atmosphere to obtain the low-oxygen titanium-containing powder; and the gas produced by the vacuum distillation is recycled by vacuum pumping to obtain the recycled lithium.

[0017] Preferably, the protective gas atmosphere is argon.

[0018] Preferably, the vacuum pumping is to a vacuum degree of < 50 Pa.

[0019] The present application provides a method for preparing low-oxygen titanium-containing powder, which comprises the following steps: deoxidizing titanium-containing powder and lithium in hydrogen or a mixed gas of hydrogen and protective gas to obtain deoxidized material; the titanium-containing powder comprises titanium powder and / or titanium alloy powder; the deoxidization temperature is 300-600 DEG C; vacuum distilling the deoxidized material to obtain low-oxygen titanium-containing powder and recycled lithium; the temperature of the vacuum distillation is 400-600 DEG C; and the oxygen content of the low-oxygen titanium-containing powder is < 1500 ppm. The present application deoxidizes titanium-containing powder (titanium powder and / or titanium alloy powder) by using lithium and hydrogen, and hydrogen reduces the stability of Ti-O solid solution, thereby realizing the thermochemical deoxidization of lithium, and a low deoxidization temperature can prevent the sintering of titanium-containing powder or damage the mechanical properties and morphology of titanium-containing powder. Then, lithium is removed by vacuum distillation, and dissolved hydrogen is also removed from titanium and titanium alloy in the vacuum distillation process. The present application can effectively reduce the oxygen content of titanium or titanium alloy to < 1500 ppm, and does not introduce hydrogen and Li, etc. as impurities to contaminate titanium or titanium alloy. Moreover, the prepared low-oxygen titanium-containing powder is not sticky, and the particles are complete, which is suitable for powder metallurgy and 3D printing.

[0020] The method has the advantages of low deoxidation temperature, clean titanium or titanium alloy powder, simple deoxidation process operation, simple process, no toxic and harmful substances, simple required equipment, low production cost, great economic and environmental benefits, and realization of production of low-oxygen titanium powder and titanium alloy powder in the industrial field. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 A preparation flowchart of the low-oxygen titanium-containing powder in the embodiments of the application is shown in the figure.

[0022] Figure 2 A real object figure of the low-oxygen titanium powder prepared in Embodiment 1 is shown in the figure. DETAILED DESCRIPTION

[0023] The application provides a preparation method of a low-oxygen titanium-containing powder, which comprises the following steps:

[0024] The titanium-containing powder and the metal lithium are deoxidized in hydrogen or a mixed gas of hydrogen and a protective gas to obtain deoxidized material; the titanium-containing powder comprises titanium powder and / or titanium alloy powder; the deoxidization temperature is 300-600°C.

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

[0026] Unless otherwise specified, the application has no special requirements for the source of the raw materials, and commercially available goods known to those skilled in the art can be used.

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

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

[0029] The deoxidization temperature in the prior art is above 800°C. Since the melting point of metal lithium is low, and the melting points of other metals are high, the deoxidization temperature needs to be above the melting point of the deoxidizer. Since other types of deoxidizers have high melting points, they can cause sintering or contamination of the titanium or titanium alloy powder, and potassium has poor deoxidization effect. Only metal lithium has the best deoxidization effect at the deoxidization temperature provided by the application. With the increase of the amount of metal lithium, the deoxidization effect can be improved, but there is no great improvement. However, metal lithium is expensive, and the deoxidization effect can meet the requirements within the amount range of metal lithium provided by the application.

[0030] As an implementation form, the particle size of the titanium-containing powder is ≤120 μm, and in particular embodiments, is 40-50 μm; the oxygen content of the titanium-containing powder is 4500-5500 ppm, and in particular embodiments, is 4650-5020 ppm; and the particle size of the lithium metal is 1-5 mm, and in particular embodiments, is 3-4 mm.

[0031] As an implementation form, 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 particular embodiments, is 10-20%; and the hydrogen or the mixed gas of hydrogen and protective gas is introduced from the bottom of the titanium-containing powder and lithium metal. The present application does not have special limitations on the flow rate of the hydrogen or the mixed gas of hydrogen and protective gas, and the gas can be introduced at a relatively small flow rate to avoid the titanium-containing powder and lithium metal from being blown away. Since the inner diameter of the gas inlet hole at the bottom of the titanium crucible is 5 mm, a relatively large flow rate will not be obtained at a relatively low flow rate of the gas.

[0032] The present application introduces the hydrogen or the mixed gas of hydrogen and protective gas from the bottom, which not only ensures that H2 can fully react with the titanium powder or titanium alloy powder, but also is beneficial to the stirring and deoxidation process and promotes the deoxidation reaction.

[0033] Hydrogen can reduce the stability of titanium-oxygen solid solution. With the increase of the amount of hydrogen, the deoxidation effect is enhanced, but when the mass concentration of hydrogen in the mixed gas exceeds 10%, the increase is not obvious.

[0034] As an implementation form, the deoxidation temperature is 300-600 °C, and in particular embodiments, is 400-600 °C; and the holding time for deoxidation is 8-32 h, and in particular embodiments, is 12-16 h.

[0035] Under the same deoxidation time, within the range set by the present application, the deoxidation effect is improved with the increase of the deoxidation temperature; under the same deoxidation temperature, the deoxidation effect is improved with the extension of the deoxidation time, and when the deoxidation time reaches 16 h, the deoxidation effect is not obviously improved with the extension of the time, and the deoxidation time range provided by the present application can ensure complete deoxidation.

[0036] As an implementation form, the heating rate for heating to the deoxidation temperature is 3-7 °C / min, and in particular embodiments, is 4-5 °C / min.

[0037] As an implementation form, the deoxidation device is a titanium crucible with a gas inlet hole at the bottom and a heating furnace, the gas inlet hole at the bottom of the titanium crucible is connected with a gas inlet pipe of the heating furnace; and the inner diameter of the gas inlet hole is 5 mm.

[0038] As an implementation form, before the deoxidation, the method further comprises: introducing hydrogen or a mixture of hydrogen and protective gas into the furnace cavity of the heating furnace until only hydrogen or the mixture of hydrogen and protective gas is in the furnace cavity, and then opening the heating furnace to heat.

[0039] As an implementation form, after the deoxidation, the method further comprises: closing the hydrogen introduction, taking out the titanium crucible after the deoxidized product is cooled to room temperature in the argon, and plugging the air hole at the bottom of the titanium crucible; and the cooling process is natural cooling.

[0040] The main reaction in 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 lithium metal.

[0041] After obtaining the deoxidized material, the method further comprises: vacuum distilling the deoxidized material to obtain low-oxygen titanium powder and recycled lithium metal.

[0042] As an implementation form, the temperature of the vacuum distillation is 400-600°C, and in a specific embodiment, the temperature is 450-550°C; and the holding time of the vacuum distillation is 6-12h, and in a specific embodiment, the holding time is 8-10h.

[0043] The temperature of the vacuum distillation is below the sintering temperature of the titanium powder (above 900°C), which can prevent the deoxidized material from sintering or damaging the mechanical properties and morphology of the deoxidized material. If the temperature is too high, the deoxidized material may crack, thereby damaging the mechanical properties or shape. In order to ensure that the lithium metal is completely volatilized, 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. The lithium removal process in the vacuum distillation can also promote the removal of dissolved hydrogen from the titanium or titanium alloy.

[0044] As an implementation form, the vacuum degree of the vacuum distillation is ≤50Pa, and in a specific embodiment, the vacuum degree is 5-30Pa.

[0045] As an implementation form, the equipment used for the vacuum distillation is a vacuum furnace; and before the vacuum distillation, the method further comprises: cleaning the vacuum furnace with argon.

[0046] As an implementation form, after the vacuum distillation, the low-oxygen titanium-containing powder is obtained by sequentially performing water washing and drying on the vacuum-distilled solid in a protective atmosphere; the gas generated in the vacuum distillation is recovered by vacuumizing to obtain the recovered metal lithium; the recovered metal lithium is used in the deoxidation process; the vacuumizing is to below 50 Pa, and in specific embodiments, to 4-10 Pa. The increase of the vacuum degree can increase the volatilization rate of the metal lithium.

[0047] As an implementation form, the protective atmosphere is argon; the reagent used in the water washing is oxygen-free deionized water; the number of times of the water washing is ≥3, and in specific embodiments, 3-5; the water washing is immersion water washing, specifically, oxygen-free deionized water is added to the vacuum-distilled solid, and stirring is continuously performed; the drying temperature is 50-70 °C, and in specific embodiments, 50-60 °C. The present application does not have a special limitation on the drying time, and the drying is performed until complete drying. Boiling can remove the dissolved gas (mainly oxygen and nitrogen) in the deionized water to obtain oxygen-free deionized water, and the water washing and drying in the protective atmosphere can prevent the gas (mainly oxygen and nitrogen) from contaminating the low-oxygen titanium-containing powder after the vacuum distillation.

[0048] As an implementation form, the present application further comprises: after the waste liquid generated in the water washing is used for water washing for multiple times, the waste liquid is used for chlorination concentration, the obtained lithium chloride is used for electrolysis to generate metal lithium and chlorine gas, the metal lithium is used in the deoxidation process, and the hydrogen chloride gas generated by the reaction of the chlorine gas and hydrogen is used in the chlorination concentration process; the multiple times are 4-7, and in specific embodiments, 5-6; the water washing is cleaning with oxygen-free pure water; the chlorination concentration is natural air-drying concentration first, the lithium hydroxide concentrated solution obtained by the concentration is chlorinated by hydrogen chloride gas to obtain lithium chloride. The present application uses the waste liquid generated in the water washing for water washing for multiple times, which can also increase the concentration of lithium ions in the waste liquid, saves energy by using natural air-drying concentration, chlorinates the concentrated lithium hydroxide by hydrogen chloride gas to obtain lithium chloride, electrolyzes the lithium chloride to generate lithium and chlorine gas, and reacts the chlorine gas with hydrogen to prepare hydrogen chloride gas used for chlorination, so that the high-value metal lithium can be recycled, and the production cost is reduced.

[0049] Figure 1The preparation process of the low-oxygen titanium-containing powder is shown in the schematic diagram of the embodiment of the present application. The titanium or titanium alloy powder and the metal lithium are deoxidized in the mixed gas of hydrogen and protective gas, the obtained deoxidized product is vacuum distilled, the metal lithium is recovered and used in the deoxidization process, the obtained titanium or titanium alloy powder is washed with water, the waste liquid is concentrated by chlorination, the obtained lithium chloride is electrolyzed to produce the metal lithium which is continuously used in the deoxidization process. Compared with the prior art, the low-temperature deoxidization is used to obtain the low-oxygen titanium-containing powder (titanium or titanium alloy powder) with optimal mechanical properties, save energy consumption, do not use acid and alkali liquid, recycle and use the metal lithium, reduce cost and increase benefit, do not produce three wastes, and is conducive to sustainable development. The method uses simple equipment manufacturing and operation, the obtained titanium or titanium alloy powder has low oxygen content, and does not introduce impurities.

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

[0051] The present application can effectively reduce the oxygen content of the titanium or titanium alloy to below 1500 ppm, and does not introduce the deoxidizer hydrogen and Li and other impurities to contaminate the titanium or titanium alloy, and the obtained low-oxygen titanium-containing powder is not sticky, the particles are complete, and is suitable for powder metallurgy and 3D printing.

[0052] The technical solutions in the present application will be described clearly and completely in combination with the embodiments in the present application, but they cannot be understood as limitations to the protection scope of the present application.

[0053] Embodiment 1

[0054] 300 g of titanium powder (oxygen content of 4650 ppm, particle size of 40-50 μm) and 60 g of lithium metal (particle size of 3-4 mm) were mixed and added to a titanium crucible with a bottom vent (inner diameter of 5 mm), the mass ratio of titanium powder to lithium metal was 5:1, the vent 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 introduce a mixture of hydrogen and argon gas from the bottom of the titanium powder and lithium metal, wherein the mass concentration of hydrogen was 10%, until only the mixture of hydrogen and argon gas was in the furnace cavity of the heating furnace, the heating furnace was opened for heating, the temperature rising rate was set to 4°C / min, the deoxidation temperature was set to 400°C, 450°C, 500°C, 550°C and 600°C respectively, and the holding time was 32 h for deoxidation, after the holding was completed, the hydrogen inlet was closed, the argon inlet was continued, and after the heating furnace was cooled to room temperature, the titanium crucible was removed, the bottom vent was plugged, and vacuum distillation was carried out in the vacuum furnace after argon washing, the distillation temperature was set to 500°C, the vacuum degree was 5 Pa, and the vacuum distillation time was 12 h, after the vacuum distillation was completed, the vacuum was extracted to 10 Pa to recover the lithium metal, the recovered lithium metal was used in the deoxidation process, and the solid after vacuum distillation was washed with oxygen-free deionized water 5 times to remove residual impurities, the water washing was immersion water washing, specifically: after adding oxygen-free deionized water to the solid after vacuum distillation, constant stirring was carried out, and drying was carried out at 50°C under high-purity argon atmosphere until complete drying, to obtain low-oxygen titanium powder.

[0055] After the waste liquid generated by the water washing was recycled for 5 times, water washing was carried out with oxygen-free pure water, natural air drying was used for concentration, lithium hydroxide concentrate obtained by concentration was chlorinated with hydrogen chloride gas, the obtained lithium chloride was electrolyzed to produce lithium metal and chlorine gas, the lithium metal was used in the deoxidation process, and the hydrogen chloride gas generated by the reaction of the chlorine gas and the hydrogen gas was used in the chlorination concentration process.

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

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

[0058]

[0059] Example 2

[0060] 300g titanium powder (oxygen content of 5020ppm, particle size of 40-50μm) and 60g of lithium metal (particle size of 3-4mm) were mixed and added into a titanium crucible with a bottom vent (inner diameter of 5mm), the mass ratio of titanium powder to lithium metal was 5:1, the vent 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 introduce a mixture of hydrogen and argon gas from the bottom of the titanium powder and lithium metal, wherein the mass concentration of hydrogen was 10%, until only the mixture of hydrogen and argon gas was in the furnace cavity of the heating furnace, the heating furnace was opened for heating, the temperature rising rate was set to 4℃ / min, the deoxidation temperature was set to 600℃, and the holding time was 4h, 8h, 12h, 16h, 24h and 32h respectively, deoxidation was carried out, after the holding was completed, the hydrogen was stopped, the argon was continuously introduced, the heating furnace was cooled to room temperature, the titanium crucible was taken out and the bottom vent was plugged, vacuum distillation was carried out in the vacuum furnace after argon washing, the distillation temperature was set to 500℃, the vacuum degree was 5Pa, and the vacuum distillation time was 12h, after the vacuum distillation was completed, the vacuum was extracted to 10Pa to recover the lithium metal, the recovered lithium metal was used in the deoxidation process, the solid after vacuum distillation was washed with oxygen-free deionized water for 5 times to remove residual impurities, the water washing was immersion method, specifically: after adding oxygen-free deionized water to the solid after vacuum distillation, constant stirring was carried out, and drying was carried out at 50℃ under high-purity argon atmosphere until complete drying, to obtain low-oxygen titanium powder.

[0061] After the waste liquid generated by the water washing was recycled for 5 times, the water washing was carried out with oxygen-free pure water, natural air drying was used for concentration, lithium hydroxide concentrate obtained by concentration was chlorinated with hydrogen chloride gas, the obtained lithium chloride was electrolyzed to produce lithium metal and chlorine gas, the lithium metal was used in the deoxidation process, and the hydrogen chloride gas generated by the reaction of chlorine gas and hydrogen was used in the chlorination concentration process.

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

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

[0064]

[0065] Example 3

[0066] 300 g of titanium alloy powder (TC4, Ti-6Al-4V, oxygen content of 4820 ppm) with particle sizes of ≤1 μm, 1-10 μm, 20-30 μm, 40-50 μm, 60-80 μm, and 100-120 μm, respectively, is mixed with 60 g of metallic lithium (particle size of 3-4 mm) to add into a titanium crucible with a bottom vent (inner diameter of 5 mm), the mass ratio of TC4 powder to metallic lithium is 5:1, the vent at the bottom of the titanium crucible is connected to a vent pipe of a heating furnace, a vent valve installed in front of a high-precision gas mass flow controller is opened to introduce a mixed gas of hydrogen and argon from the bottom of the titanium powder and the metallic lithium, the mass concentration of hydrogen is 10%, until only the mixed gas of hydrogen and argon is in the furnace cavity of the heating furnace, the heating furnace is opened for heating, the temperature rising rate is set to 4°C / min, the deoxidization temperature is set to 550°C, and the holding time is 12 h, deoxidization is performed, after the holding is completed, the introduction of hydrogen is stopped, argon is continuously introduced, the heating furnace is cooled to room temperature, the titanium crucible is taken out, the vent at the bottom is blocked, vacuum distillation is performed in a vacuum furnace after argon washing, the distillation temperature is set to 500°C, the vacuum degree is 5 Pa, the vacuum distillation time is 12 h, after the vacuum distillation is completed, the vacuum is extracted to 10 Pa to recover the metallic lithium, the recovered metallic lithium is used in the deoxidization process, the solid after the vacuum distillation is washed with oxygen-free deionized water 5 times to remove residual impurities, the water washing is immersion water washing, specifically, oxygen-free deionized water is added to the solid after the vacuum distillation, stirring is continuously performed, and the solid is dried to complete dryness at 50°C under a high-purity argon atmosphere, low-oxygen titanium alloy powder is obtained;

[0067] After the waste liquid generated in the water washing is recycled 5 times, the water washing is performed with oxygen-free pure water, natural air-drying is first used for concentration, lithium hydroxide concentrate obtained by the concentration is chlorinated with hydrogen chloride gas, the obtained lithium chloride is electrolyzed to generate metallic lithium and chlorine gas, the metallic lithium is used in the deoxidization process, and the hydrogen chloride gas generated by the reaction of the chlorine gas and the hydrogen gas is used in the chlorination and concentration process.

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

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

[0070]

[0071] As shown in the above table, the oxygen content of the low-oxygen titanium powder or low-oxygen titanium alloy powder obtained in Examples 1-3 is generally 900-1500 ppm, the yield of the low-oxygen titanium powder or low-oxygen titanium alloy powder is more than 99%, and the recovery rate of the metallic lithium is more than 90%.

[0072] Figure 2The low-oxygen titanium powder prepared in Example 1 is shown in the figure. As can be seen from the figure, the low-oxygen titanium powder has good particle uniformity, and the low-oxygen titanium powder is spherical and complete under a microscope, and the powders are not adhered to each other. In the present application, the deoxidization temperature is low, the titanium powder will not be sintered, and the titanium powder particles will not be deformed.

[0073] Although the above embodiment has made a detailed description of the present application, it is only a part of the embodiments of the present application but not all the embodiments, and other embodiments can be obtained according to the present embodiment without creativity, which all belong to the protection scope of the present application.

Claims

1. A method for preparing low-oxygen titanium-containing powder, characterized in that, Includes the following steps: Titanium-containing powder and metallic lithium are deoxidized in hydrogen or a mixture of hydrogen and protective gas to obtain deoxidized material; the titanium-containing powder includes titanium powder and / or titanium alloy powder; the deoxidation temperature is 300-600℃. The deoxygenated material is subjected to vacuum distillation to obtain low-oxygen titanium-containing powder and recovered metallic lithium; the temperature of the vacuum distillation is 400-600℃; the oxygen content of the low-oxygen titanium-containing powder is <1500ppm.

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 deoxygenation holding time is 8–32 hours.

4. The preparation method according to claim 1, characterized in that, The vacuum distillation process is carried out for 6 to 12 hours.

5. The preparation method according to claim 1 or 3, characterized in that, The heating rate to the deoxygenation 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 mixture 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 vacuum distillation, the process further includes: washing and drying the solid obtained by vacuum distillation in a protective atmosphere to obtain the low-oxygen titanium-containing powder; and recovering the gas generated by vacuum distillation by vacuum extraction to obtain the recovered lithium metal.

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 then reduced to below 50 Pa.

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