Spherical nanometer titanium dioxide for lithium ion battery and preparation method thereof

By using sponge titanium or metallic titanium powder and chloride salts as raw materials, spherical nano-titanium dioxide was prepared at low temperature, solving the conductivity and diffusion problems of existing lithium-ion battery materials. This resulted in high-purity nano-titanium dioxide with high oxygen vacancy concentration, simplifying the process and reducing costs.

CN122212239APending Publication Date: 2026-06-16WUHAN UNIV OF SCI & TECH +1

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
WUHAN UNIV OF SCI & TECH
Filing Date
2026-04-23
Publication Date
2026-06-16

AI Technical Summary

Technical Problem

Existing nano-TiO2 materials for lithium-ion batteries suffer from low electronic conductivity and small lithium-ion diffusion coefficient, resulting in high charge transport resistance and insufficient rate performance. Furthermore, existing preparation methods are complex, costly, and cause serious environmental pollution.

Method used

Spherical nano-titanium dioxide was prepared by using sponge titanium or metallic titanium powder as the titanium source, potassium chloride, sodium chloride, lithium chloride, etc. as co-solvents, and potassium perchlorate as the oxygen source, and keeping it at 600~800℃ for 1~6h under flowing gas. Then it was washed with distilled water and dried.

Benefits of technology

The prepared spherical nano-titanium dioxide for lithium-ion batteries has high purity and high oxygen vacancy concentration. The process is simple, low-cost, and environmentally friendly, and the purity and particle size uniformity are good.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application relates to a spherical nanometer titanium dioxide for lithium ion batteries and a preparation method thereof. The technical scheme is as follows: 15-35 wt% of a titanium source, 40-70 wt% of a cosolvent and 10-30 wt% of potassium perchlorate are mixed to obtain a mixture. The mixture is placed in a high-temperature atmosphere furnace, and is first heated to 300-500 DEG C under the condition of flowing gas, and then heated to 600-800 DEG C, and is naturally cooled after heat preservation to obtain a reaction product. The reaction product is soaked in distilled water I, washed with distilled water II, and is subjected to solid-liquid separation; the obtained washing liquid is dried to serve as the cosolvent, and the obtained solid is dried to prepare the spherical nanometer titanium dioxide for lithium ion batteries. The application has the characteristics of simple process, low cost, environmental friendliness and easy process control, and the prepared spherical nanometer titanium dioxide for lithium ion batteries is high in purity and high in oxygen vacancy concentration.
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Description

Technical Field

[0001] This invention belongs to the field of spherical nano-titanium dioxide technology. Specifically, it relates to a spherical nano-titanium dioxide for lithium-ion batteries and its preparation method. Background Technology

[0002] Nano-titanium dioxide (TiO2) is considered a potential anode material for lithium-ion batteries due to its abundant resources, low cost, environmental friendliness, high chemical inertness, and good safety.

[0003] Currently, the practical application of nano-TiO2 in lithium-ion batteries still faces challenges such as low electronic conductivity and small lithium-ion diffusion coefficient. These problems lead to high charge transport resistance and insufficient rate performance of TiO2 during charging and discharging, necessitating breakthroughs through material design and modification. Jiang Jiajie et al. (Jiang Jiajie, Xie Xinyuan, Li Fengyu. Amorphous titanium dioxide modified titanium dioxide photonic crystal electrode and its photoelectric properties [J]. Journal of the Chinese Ceramic Society, 2025, 53(1): 95-101.) summarized various preparation methods in their research progress on spherical nano-titanium dioxide, including solvothermal, hydrothermal, template, and electrochemical deposition methods. However, they did not point out the method of controlling the solubility of titanium powder through molten salt and in-situ contact with oxygen to introduce vacancy defects and shape the surface of TiO2 powder. Therefore, the study of TiO2 powder has attracted the attention of those skilled in the art.

[0004] For example, Li Binghui et al. (Li Binghui, Gong Xiannian, Su Jing, et al. Synthesis of nano-titanium dioxide anode material for lithium-ion batteries by ionic liquid[J]. Inorganic Salt Industry, 2017, 49(1):66-69.) prepared nano-titanium dioxide for lithium-ion batteries in a urea-choline chloride ionic liquid system. Although the prepared material has good electrochemical performance, the preparation process is complicated and the cost is high.

[0005] For example, Sun Yansheng (Sun Yansheng. Preparation and Electrochemical Performance Study of Oxygen Vacancy-Containing Titanium Dioxide-Based Anode Materials [D]. Jiangsu: Nanjing University of Aeronautics and Astronautics, 2018.) used a hydrothermal method combined with hydrothermal reduction of hydrazine hydrate aqueous solutions of different concentrations to prepare TiO2 containing different oxygen vacancy concentrations. 2-x Although TiO2 containing oxygen vacancies was found in the anode material... 2-x It has better electrochemical performance, but the prepared product has a low oxygen vacancy concentration.

[0006] The patented technology "A method for preparing high-purity titanium dioxide" (CN121361827A) uses titanium tetrachloride hydrolysis to prepare titanium dioxide. The product has high purity, but the yield is only about 90% and the powder agglomeration is serious.

[0007] The patented technology "A method for preparing high-purity titanium dioxide" (CN117819598A) uses titanium tetrachloride and hydrochloric acid as raw materials to prepare high-purity titanium dioxide through two hydrolysis processes. Although the hydrolysis rate is high, the preparation process is complex, the process is not easy to control, and the waste liquid is easy to pollute the environment.

[0008] The patented technologies "A High-Purity Spherical Titanium Dioxide and Its Preparation Method" (CN118929745A) and "A High-Purity Spherical Titanium Dioxide and Its Preparation Method" (CN118929745B) use titanium-containing blast furnace slag as raw material. Impurities are removed by complexing agents, surface-active agents and dispersants, and the powder particles are shaped at the same time. Although this achieves the resource utilization of industrial waste, the prepared products have high impurity content and low purity. Summary of the Invention

[0009] The present invention aims to overcome the defects of the prior art and to provide a simple, low-cost, environmentally friendly, and easy-to-control process for preparing spherical nano-titanium dioxide for lithium-ion batteries with high purity and high oxygen vacancy concentration.

[0010] To achieve the above objectives, the specific steps of the technical solution adopted by the present invention are as follows: Step 1: Mix 15-35 wt% of titanium source, 40-70 wt% of co-solvent and 10-30 wt% of potassium perchlorate to obtain a mixture.

[0011] Step 2: Place the mixture in a high-temperature atmosphere furnace, and under flowing gas conditions, raise the temperature to 300~500℃ for the first time, raise the temperature to 600~800℃ for the second time, hold the temperature for 1~6 hours, and then cool naturally to obtain the reaction product.

[0012] Step 3: Soak the reaction product in distilled water I for 1-20 hours, wash it with distilled water II 3-5 times, and separate the solid and liquid. Then dry the obtained washing liquid as a co-solvent, and then dry the obtained solid to obtain spherical nano titanium dioxide for lithium-ion batteries.

[0013] The titanium source is sponge titanium or metallic titanium powder, with a purity of 95~99.9wt% and a particle size of 0.1~200μm.

[0014] The co-solvent is one or more of potassium chloride, sodium chloride, and lithium chloride, with a purity ≥99wt% and a particle size ≤0.075mm.

[0015] The potassium perchlorate has a purity of 99 wt% or higher and a particle size of ≤0.075 mm.

[0016] The rate of the first heating is 1~2℃ / min.

[0017] The rate of the second heating is 3~5℃ / min.

[0018] The flowing gas is argon or oxygen, and the purity of the flowing gas is ≥99.9wt%.

[0019] The temperature of the distilled water is 50~100℃; Distilled water II is the same as distilled water I.

[0020] The drying temperature is 100~220℃, and the drying time is 12~36h.

[0021] By adopting the above technical solution, the present invention has the following advantages compared with the prior art: This invention uses sponge titanium or metallic titanium powder as the titanium source, one or more of potassium chloride, sodium chloride, and lithium chloride as a co-solvent, and potassium perchlorate as the oxygen source. The reaction is carried out under flowing gas at 600-800°C for 1-6 hours to obtain the reaction product. The product is then washed with distilled water, and the resulting solid is dried to obtain spherical nano-titanium dioxide for lithium-ion batteries. The resulting liquid is dried and used as a co-solvent. The titanium source, co-solvent, and potassium perchlorate used in this invention are all commercially available, thus the process is simple, low-cost, has a high raw material reusability rate, and is easy to control.

[0022] The spherical nano-titanium dioxide prepared by this invention has high purity and high oxygen vacancy concentration for lithium-ion batteries. On the one hand, titanium dioxide easily loses lattice oxygen in a low oxygen potential environment at high temperatures, spontaneously forming oxygen vacancies; on the other hand, the molten chloride salt extracts oxygen ions from the generated titanium dioxide lattice, creating a large number of oxygen vacancies. Both of these factors combined result in a high oxygen vacancy concentration in the prepared spherical nano-titanium dioxide for lithium-ion batteries.

[0023] The co-solvent used in this invention is readily soluble in distilled water, and the reaction product can be washed with distilled water. The washing liquid after solid-liquid separation can be evaporated and reused as a co-solvent.

[0024] The spherical nano-titanium dioxide powder for lithium-ion batteries prepared by the molten salt method at low temperature has high purity. Because the eutectic point of the flux is 400~600℃, it can generate a liquid phase environment, which improves the dissolution and reaction rate of the titanium source. Furthermore, the powder obtained by the molten salt method has a uniform structure, and the spherical morphology of the product is uniform with good crystal development and a diameter of about 50~100nm.

[0025] This invention uses chloride salt as a co-solvent and heats the mixture to 300-500°C at a rate of 1-2°C / min. This causes the co-solvent to form a liquid phase and promotes the dissolution of the titanium source in the liquid phase. This significantly reduces the reaction temperature and allows for direct contact with the oxygen source during subsequent heating. The process is simple, and the resulting spherical nano-titanium dioxide for lithium-ion batteries has high purity.

[0026] The spherical nano-titanium dioxide for lithium-ion batteries prepared in this invention was tested and found to have a purity of ≥99.5 wt%; D 50 The particle size is ≤100nm. The purity of the product manufactured in this invention is detected by gas chromatography, and the D50 particle size is detected by laser particle size distribution.

[0027] Therefore, the present invention has the characteristics of simple process, low cost, environmental friendliness and easy process control, and the prepared spherical nano titanium dioxide for lithium-ion batteries has high purity and high oxygen vacancy concentration. Attached Figure Description

[0028] Figure 1 The XRD pattern of a spherical nano-titanium dioxide for lithium-ion batteries prepared according to the present invention; Figure 2 for Figure 1 The image shown is a SEM image of spherical nano-titanium dioxide used in lithium-ion batteries. Detailed Implementation Plan The present invention will be further described below with reference to the accompanying drawings and specific embodiments, but this is not intended to limit the scope of protection thereof.

[0029] A spherical nano-titanium dioxide for lithium-ion batteries and its preparation method. The preparation method described in this specific embodiment is as follows: Step 1: Mix 15-35 wt% of titanium source, 40-70 wt% of co-solvent and 10-30 wt% of potassium perchlorate to obtain a mixture.

[0030] Step 2: Place the mixture in a high-temperature atmosphere furnace, and under flowing gas conditions, raise the temperature to 300~500℃ for the first time, raise the temperature to 600~800℃ for the second time, hold the temperature for 1~6 hours, and then cool naturally to obtain the reaction product.

[0031] Step 3: Soak the reaction product in distilled water I for 1-20 hours, wash it with distilled water II 3-5 times, and separate the solid and liquid. Then dry the obtained washing liquid as a co-solvent, and then dry the obtained solid to obtain spherical nano titanium dioxide for lithium-ion batteries.

[0032] The titanium source is sponge titanium or metallic titanium powder, and the purity of the titanium source is 95~99.9wt%.

[0033] The co-solvent is one or more of potassium chloride, sodium chloride, and lithium chloride, and the purity of the co-solvent is ≥99wt%.

[0034] The potassium perchlorate has a purity of 99 wt% or higher.

[0035] The rate of the first heating is 1~2℃ / min.

[0036] The rate of the second heating is 3~5℃ / min.

[0037] The flowing gas is argon or oxygen, and the purity of the flowing gas is ≥99.9 Vol.

[0038] The temperature of distilled water I is 50~100℃; distilled water I is the same as distilled water II.

[0039] The drying temperature is 100~220℃, and the drying time is 12~36h.

[0040] In this specific implementation: The particle size of the titanium source is 0.1~200μm.

[0041] The particle size of the cosolvent is ≤0.075mm.

[0042] The potassium perchlorate has a particle size ≤0.075mm.

[0043] Distilled water II is the same as distilled water I.

[0044] The details will not be repeated in the examples.

[0045] Example 1 A spherical nano-titanium dioxide for lithium-ion batteries and its preparation method. The preparation method described in this embodiment is as follows: Step 1: Mix 15wt% titanium source, 65wt% co-solvent and 20wt% potassium perchlorate to obtain a mixture.

[0046] Step 2: Place the mixture in a high-temperature atmosphere furnace, and under flowing gas conditions, raise the temperature to 300°C for the first time, raise it to 600°C for the second time, hold it at that temperature for 1 hour, and then let it cool naturally to obtain the reaction product.

[0047] Step 3: Soak the reaction product in distilled water I for 1 hour, wash it three times with distilled water II, and separate the solid and liquid. Then dry the obtained washing liquid as a co-solvent, and then dry the obtained solid to obtain spherical nano-titanium dioxide for lithium-ion batteries.

[0048] The titanium source is metallic titanium powder with a purity of 98 wt%.

[0049] The co-solvent is potassium chloride, and the purity of the co-solvent is 99.5 wt%.

[0050] The purity of the potassium perchlorate is 99.2 wt%.

[0051] The rate of the first heating is 1℃ / min.

[0052] The rate of the second heating is 3°C / min.

[0053] The flowing gas is oxygen, and the purity of the flowing gas is 99.9 Vol.

[0054] The temperature of the distilled water I is 100℃.

[0055] The drying temperature is 100℃ and the drying time is 36 hours.

[0056] The spherical nano-titanium dioxide for lithium-ion batteries prepared in this embodiment was tested and found to have a purity of 99.5 wt%; D 50 The particle size is 50 nm.

[0057] Example 2 A spherical nano-titanium dioxide for lithium-ion batteries and its preparation method. The preparation method described in this embodiment is as follows: Step 1: Mix 20wt% titanium source, 55wt% co-solvent and 25wt% potassium perchlorate to obtain a mixture.

[0058] Step 2: Place the mixture in a high-temperature atmosphere furnace, and under flowing gas conditions, raise the temperature to 350°C for the first time, raise it to 650°C for the second time, hold it at that temperature for 2 hours, and then allow it to cool naturally to obtain the reaction product.

[0059] Step 3: Soak the reaction product in distilled water I for 5 hours, wash it 4 times with distilled water II, and separate the solid and liquid. Then dry the obtained washing liquid as a co-solvent, and then dry the obtained solid to obtain spherical nano titanium dioxide for lithium-ion batteries.

[0060] The titanium source is sponge titanium, and the purity of the titanium source is 99wt%.

[0061] The co-solvent is sodium chloride, and the purity of the co-solvent is 99.6 wt%.

[0062] The purity of the potassium perchlorate is 99.5 wt%.

[0063] The rate of the first heating is 1.3℃ / min.

[0064] The second heating rate is 3.5℃ / min.

[0065] The flowing gas is oxygen, and the purity of the flowing gas is 99.99 Vol.

[0066] The temperature of the distilled water I is 85℃.

[0067] The drying temperature is 150℃ and the drying time is 30 hours.

[0068] The spherical nano-titanium dioxide for lithium-ion batteries prepared in this embodiment was tested and found to have a purity of 99.6 wt%; D 50 The particle size is 90.5 nm.

[0069] Example 3 A spherical nano-titanium dioxide for lithium-ion batteries and its preparation method. The preparation method described in this embodiment is as follows: Step 1: Mix 25wt% titanium source, 45wt% co-solvent and 30wt% potassium perchlorate to obtain a mixture.

[0070] Step 2: Place the mixture in a high-temperature atmosphere furnace, and under flowing gas conditions, raise the temperature to 400°C for the first time, raise it to 700°C for the second time, hold it at that temperature for 3 hours, and then let it cool naturally to obtain the reaction product.

[0071] Step 3: Soak the reaction product in distilled water I for 10 hours, wash it 5 times with distilled water II, and separate the solid and liquid. Then dry the obtained washing liquid as a co-solvent, and then dry the obtained solid to obtain spherical nano titanium dioxide for lithium-ion batteries.

[0072] The titanium source is metallic titanium powder with a purity of 99.5 wt%.

[0073] The co-solvent is lithium chloride, and the purity of the co-solvent is 99 wt%.

[0074] The purity of the potassium perchlorate is 99.6 wt%.

[0075] The rate of the first heating is 1.5℃ / min.

[0076] The rate of the second heating is 4°C / min.

[0077] The flowing gas is argon, and the purity of the flowing gas is 99.999 Vol.

[0078] The temperature of the distilled water I is 70°C.

[0079] The drying temperature is 180℃, and the drying time is 25 hours.

[0080] The spherical nano-titanium dioxide for lithium-ion batteries prepared in this embodiment was tested and found to have a purity of 99.8 wt%; D 50 The particle size is 95.2 nm.

[0081] Example 4 A spherical nano-titanium dioxide for lithium-ion batteries and its preparation method. The preparation method described in this embodiment is as follows: Step 1: Mix 30wt% titanium source, 60wt% co-solvent and 10wt% potassium perchlorate to obtain a mixture.

[0082] Step 2: Place the mixture in a high-temperature atmosphere furnace, and under flowing gas conditions, raise the temperature to 450°C for the first time, raise it to 750°C for the second time, hold it at that temperature for 4 hours, and then allow it to cool naturally to obtain the reaction product.

[0083] Step 3: Soak the reaction product in distilled water I for 15 hours, wash it 4 times with distilled water II, and separate the solid and liquid. Then dry the obtained washing liquid as a co-solvent, and then dry the obtained solid to obtain spherical nano titanium dioxide for lithium-ion batteries.

[0084] The titanium source is sponge titanium, and the purity of the titanium source is 99.6 wt%.

[0085] The co-solvent is a mixture of potassium chloride and sodium chloride, and the purity of the co-solvent is 99.5 wt%.

[0086] The purity of the potassium perchlorate is 99.7 wt%.

[0087] The rate of the first heating is 1.8℃ / min.

[0088] The second heating rate is 4.5℃ / min.

[0089] The flowing gas is oxygen, and the purity of the flowing gas is 99.99 Vol.

[0090] The temperature of the distilled water I is 60°C.

[0091] The drying temperature is 200℃, and the drying time is 20 hours.

[0092] The spherical nano-titanium dioxide for lithium-ion batteries prepared in this embodiment was tested and found to have a purity of 99.9 wt%; D 50 The particle size is 98.1 nm.

[0093] Example 5 A spherical nano-titanium dioxide for lithium-ion batteries and its preparation method. The preparation method described in this embodiment is as follows: Step 1: Mix 35wt% titanium source, 50wt% co-solvent and 15wt% potassium perchlorate to obtain a mixture.

[0094] Step 2: Place the mixture in a high-temperature atmosphere furnace, and under flowing gas conditions, raise the temperature to 500°C for the first time, raise it to 800°C for the second time, hold it at that temperature for 6 hours, and then allow it to cool naturally to obtain the reaction product.

[0095] Step 3: Soak the reaction product in distilled water I for 20 hours, wash it 5 times with distilled water II, and separate the solid and liquid. Then dry the obtained washing liquid as a co-solvent, and then dry the obtained solid to obtain spherical nano titanium dioxide for lithium-ion batteries.

[0096] The titanium source is metallic titanium powder with a purity of 99.8 wt%.

[0097] The co-solvent is a mixture of potassium chloride and lithium chloride, and the purity of the co-solvent is 99.6 wt%.

[0098] The purity of the potassium perchlorate is 99.8 wt%.

[0099] The rate of the first heating is 2°C / min.

[0100] The rate of the second heating is 5°C / min.

[0101] The flowing gas is oxygen, and the purity of the flowing gas is 99.999 Vol.

[0102] The temperature of the distilled water I is 50°C.

[0103] The drying temperature is 220℃, and the drying time is 12 hours.

[0104] The spherical nano-titanium dioxide for lithium-ion batteries prepared in this embodiment was tested and found to have a purity of 99.9 wt%; D 50 The particle size is 100 nm.

[0105] Example 6 A spherical nano-titanium dioxide for lithium-ion batteries and its preparation method. This embodiment is identical to Example 1 except as described below.

[0106] Step 1: Mix 32wt% titanium source, 40wt% co-solvent and 28wt% potassium perchlorate to obtain a mixture.

[0107] The co-solvent is a mixture of sodium chloride and lithium chloride, and the purity of the co-solvent is 99.3 wt%.

[0108] The spherical nano-titanium dioxide for lithium-ion batteries prepared in this embodiment was tested and found to have a purity of 99.7 wt%; D 50 The particle size is 85.3 nm.

[0109] Example 7 A spherical nano-titanium dioxide for lithium-ion batteries and its preparation method. This embodiment is identical to Example 2 except as described below.

[0110] Step 1: Mix 18wt% of titanium source, 70wt% of co-solvent and 12wt% of potassium perchlorate to obtain a mixture.

[0111] The co-solvent is a mixture of potassium chloride, sodium chloride and lithium chloride, and the purity of the co-solvent is 99.7 wt%.

[0112] The spherical nano-titanium dioxide for lithium-ion batteries prepared in this embodiment was tested and found to have a purity of 99.9 wt%; D 50 The particle size is 90.7 nm.

[0113] This specific implementation method has the following advantages compared with the prior art: This specific embodiment uses sponge titanium or metallic titanium powder as the titanium source, one or more of potassium chloride, sodium chloride, and lithium chloride as the co-solvent, and potassium perchlorate as the oxygen source. The reaction is carried out under flowing gas at 600-800°C for 1-6 hours to obtain the reaction product. The product is then washed with distilled water, and the resulting solid is dried to obtain spherical nano-titanium dioxide for lithium-ion batteries. The resulting liquid is dried and used as a co-solvent. The titanium source, co-solvent, and potassium perchlorate used in this specific embodiment are all commercially available, thus the process is simple, low-cost, has a high raw material reuse rate, and is easy to control.

[0114] The spherical nano-titanium dioxide prepared in this specific embodiment has high purity and high oxygen vacancy concentration for lithium-ion batteries. On the one hand, titanium dioxide easily loses lattice oxygen in a low oxygen potential environment at high temperatures, spontaneously forming oxygen vacancies; on the other hand, the molten chloride salt extracts oxygen ions from the generated titanium dioxide lattice, creating a large number of oxygen vacancies. Both of these factors combined result in a high oxygen vacancy concentration in the prepared spherical nano-titanium dioxide for lithium-ion batteries.

[0115] The co-solvent used in this specific embodiment is readily soluble in distilled water, and the reaction product can be washed with distilled water. The washing liquid after solid-liquid separation can be evaporated and reused as a co-solvent. This specific embodiment uses the molten salt method to synthesize spherical nano-titanium dioxide powder with high purity at low temperature. Because the eutectic point of the co-solvent is 400~600℃, it can generate a liquid phase environment, which improves the dissolution of the titanium source and the reaction rate.

[0116] The spherical nano-titanium dioxide for lithium-ion batteries prepared in this specific embodiment is shown in the attached figure. Figure 1 The XRD pattern of the spherical nano-titanium dioxide for lithium-ion batteries prepared in Example 2; Figure 2 for Figure 1 The image shown is a SEM image of spherical nano-titanium dioxide used in lithium-ion batteries. Figure 1 It can be seen that the prepared product contains only the titanium dioxide phase, indicating that the titanium source has completely reacted to form titanium dioxide. Figure 2 It is evident that the product exhibits a uniform structure, consistent spherical morphology, and well-developed crystals with a diameter of approximately 50-100 nm. In this specific embodiment, chloride salt is used as a co-solvent, and the mixture is heated to 300-500°C at a rate of 1-2°C / min. This allows the co-solvent to form a liquid phase and promotes the dissolution of the titanium source in the liquid phase. This significantly reduces the reaction temperature and allows for direct contact with the oxygen source during subsequent heating. The process is simple, and the resulting spherical nano-titanium dioxide for lithium-ion batteries has high purity.

[0117] The spherical nano-titanium dioxide for lithium-ion batteries prepared in this specific embodiment was tested and found to have a purity of ≥99.5 wt%; D 50 The particle size is ≤100nm. The purity of the product prepared in this specific embodiment is detected by gas chromatography, and the D50 particle size is detected by laser particle size distribution.

[0118] Therefore, this specific embodiment has the characteristics of simple process, low cost, environmental friendliness and easy process control, and the prepared spherical nano titanium dioxide for lithium-ion batteries has high purity and high oxygen vacancy concentration.

Claims

1. A method for preparing spherical nano-titanium dioxide for lithium-ion batteries, characterized in that... The steps of the preparation method are as follows: Step 1: Mix 15-35 wt% of titanium source, 40-70 wt% of co-solvent and 10-30 wt% of potassium perchlorate to obtain a mixture; Step 2: Place the mixture in a high-temperature atmosphere furnace, and under flowing gas conditions, raise the temperature to 300~500℃ for the first time, raise the temperature to 600~800℃ for the second time, hold the temperature for 1~6 hours, and cool naturally to obtain the reaction product; Step 3: Soak the reaction product in distilled water I for 1-20 hours, wash it with distilled water II 3-5 times, and separate the solid and liquid. Then dry the obtained washing liquid as a co-solvent, and then dry the obtained solid to obtain spherical nano titanium dioxide for lithium-ion batteries.

2. The method for preparing spherical nano-titanium dioxide for lithium-ion batteries according to claim 1, characterized in that, The titanium source is sponge titanium or metallic titanium powder, with a purity of 95~99.9wt% and a particle size of 0.1~200μm.

3. The method for preparing spherical nano-titanium dioxide for lithium-ion batteries according to claim 1, characterized in that, The co-solvent is one or more of potassium chloride, sodium chloride, and lithium chloride, and the purity of the co-solvent is ≥99wt%, and the particle size of the co-solvent is ≤0.075mm.

4. The method for preparing spherical nano-titanium dioxide for lithium-ion batteries according to claim 1, characterized in that, The potassium perchlorate has a purity of 99 wt% or higher and a particle size of ≤0.075 mm.

5. The method for preparing spherical nano-titanium dioxide for lithium-ion batteries according to claim 1, characterized in that, The rate of the first heating is 1~2℃ / min.

6. The method for preparing spherical nano-titanium dioxide for lithium-ion batteries according to claim 1, characterized in that, The rate of the second heating is 3~5℃ / min.

7. The method for preparing spherical nano-titanium dioxide for lithium-ion batteries according to claim 1, characterized in that, The flowing gas is argon or oxygen, and the purity of the flowing gas is ≥99.9wt%.

8. The method for preparing spherical nano-titanium dioxide for lithium-ion batteries according to claim 1, characterized in that, The temperature of distilled water I is 50~100℃; distilled water II is the same as distilled water I.

9. The method for preparing spherical nano-titanium dioxide for lithium-ion batteries according to claim 1, characterized in that, The drying temperature is 100~220℃, and the drying time is 12~36h.

10. A spherical nano-titanium dioxide for lithium-ion batteries, characterized in that... The spherical nano-titanium dioxide for lithium-ion batteries is prepared according to the preparation method of spherical nano-titanium dioxide for lithium-ion batteries according to any one of claims 1 to 9.