CN113921811A - Method for preparing doped lithium titanate, doped lithium titanate and lithium ion battery cathode material with doped lithium titanate - Google Patents

Method for preparing doped lithium titanate, doped lithium titanate and lithium ion battery cathode material with doped lithium titanate Download PDF

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Publication number
CN113921811A
CN113921811A CN202111058178.8A CN202111058178A CN113921811A CN 113921811 A CN113921811 A CN 113921811A CN 202111058178 A CN202111058178 A CN 202111058178A CN 113921811 A CN113921811 A CN 113921811A
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lithium titanate
doped
doped lithium
precursor
polyethylene glycol
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杨龙奎
王荣荣
刘喆
李倩倩
雷磊
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Yinlong New Energy Co Ltd
Northern Altair Nanotechnologies Co Ltd
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Yinlong New Energy Co Ltd
Northern Altair Nanotechnologies Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention provides a method for preparing doped lithium titanate, the doped lithium titanate and a lithium ion battery cathode material with the doped lithium titanate, and the method for preparing the doped lithium titanate comprises the following steps: using a mixed solution of polyethylene glycol and water as a hydrolysis solvent of titanyl sulfate; adding titanyl sulfate into a hydrolysis solvent, adding a compound containing metal ions into the hydrolysis solvent, and allowing the metal ions in the compound containing metal ions to participate in the hydrolysis reaction of the titanyl sulfate to obtain a precursor comprising doped metatitanic acid and polyethylene glycol; and mixing the precursor with a lithium source, and carrying out chemical reaction on the precursor and the lithium source to obtain the doped lithium titanate. By adopting the technical scheme, the conductivity of the prepared doped lithium titanate is effectively improved.

Description

Method for preparing doped lithium titanate, doped lithium titanate and lithium ion battery cathode material with doped lithium titanate
Technical Field
The invention relates to the technical field of lithium titanate preparation processes, in particular to a method for preparing doped lithium titanate, the doped lithium titanate and a lithium ion battery cathode material with the doped lithium titanate.
Background
In the prior art, the raw materials for preparing lithium titanate comprise a lithium source and a titanium source, and titanium dioxide is often used as the titanium source in the raw materials for preparing lithium titanate with a spinel structure. The existing titanium dioxide on the market is mainly used in the fields of paint, coating, fine ceramics and the like, most of the titanium dioxide is pigment-grade rutile titanium dioxide, and the rutile titanium dioxide has mature process and good batch stability. Titanium dioxide special for lithium batteries is usually anatase type, the market amount of anatase type titanium dioxide is small, the process maturity and the batch stability are poorer than those of rutile type titanium dioxide, so that the produced lithium titanate has customization requirements on titanium dioxide, the manufacturing cost of lithium titanate is high, and the exertion of the electrochemical properties of lithium titanate is obviously influenced by selecting different titanium dioxide as a titanium source.
Metatitanic acid is an intermediate product in the technical process of producing titanium dioxide by a sulfuric acid method, and metatitanic acid is directly used as a titanium source of a lithium battery cathode material lithium titanate, so that the method has the following advantages: 1. the sintering process from metatitanic acid to titanium dioxide is omitted, so that the production cost is reduced; 2. compared with titanium dioxide, metatitanic acid has higher activity, and the synthesized lithium titanate has lower reaction temperature, thereby effectively reducing the production energy consumption; 3. the market selection is richer, and the raw materials are more easily obtained.
Disclosure of Invention
The invention mainly aims to provide a method for preparing doped lithium titanate, the doped lithium titanate and a lithium ion battery cathode material with the doped lithium titanate, so as to solve the problem that prepared lithium titanate in the prior art is poor in conductivity.
In order to achieve the above object, according to an aspect of the present invention, there is provided a method of preparing doped lithium titanate, including: using a mixed solution of polyethylene glycol and water as a hydrolysis solvent of titanyl sulfate; adding titanyl sulfate into the hydrolysis solvent, adding a compound containing metal ions into the hydrolysis solvent, and allowing the metal ions in the compound containing metal ions to participate in the hydrolysis reaction of the titanyl sulfate to obtain a precursor containing doped metatitanic acid and polyethylene glycol; and mixing the precursor with a lithium source, and carrying out chemical reaction on the precursor and the lithium source to obtain the doped lithium titanate.
Further, the compound containing the metal ions is one or more of an oxide of the metal M, a hydroxide of the metal M, a sulfate of the metal M and a sulfate oxide of the metal M, wherein M is one or a combination of more of Ag, Au, Cu, Zr, Mg, Nb, Ca, V, Sr and Mo.
Further, the doped metatitanic acid has a structural formula H2TixM1-xO3Wherein the value range of x is 0.0-0.99.
Further, the mass ratio of the polyethylene glycol to the water in the mixed solution of the polyethylene glycol and the water is 9: 1-1: 9.
Furthermore, the physical diameter of the primary particle of the doped lithium titanate is between 100 and 400 nm.
Further, the step of chemically reacting the precursor and the lithium source comprises: and mixing the precursor and a lithium source, ball-milling, and sintering the obtained solid mixture at 730-750 ℃ in an inert atmosphere to obtain the doped lithium titanate.
Further, after the step of hydrolyzing, the method further comprises: and washing a product obtained by the hydrolysis reaction by using a mixed solution of polyethylene glycol and water, and then filtering and drying to obtain a precursor.
Further, after the hydrolysis reaction step and before the washing step, the method further comprises: heating the reaction slurry obtained by the hydrolysis reaction to 60-80 ℃, adding ammonia water for neutralization, controlling the pH value of a neutralization end point to be 6.0-7.0, uniformly stirring, curing for 0.5-2 h, collecting the cured product, and washing; the drying process adopts a spray drying mode.
According to another aspect of the invention, a doped lithium titanate is provided, which is prepared by the method.
According to another aspect of the invention, a lithium ion battery negative electrode material is provided, which comprises the doped lithium titanate.
By applying the technical scheme of the invention, the mixed solution of polyethylene glycol and water is used as a hydrolysis solvent of titanyl sulfate, and the polyethylene glycol can prevent excessive agglomeration of doped metatitanic acid generated after hydrolysis of titanyl sulfate, so that the prepared doped lithium titanate has smaller primary particles, and further the ion migration path of the doped lithium titanate is shorter, and the lithium ion migration rate is higher; polyethylene glycol is contained in the doped lithium titanate as a carbon source, so that the conductivity of the doped lithium titanate is improved. Meanwhile, a compound of specific metal ions is added into a hydrolysis solvent, so that the metal ions participate in titanyl sulfate hydrolysis reaction, and the metal ions are uniformly doped into the doped metatitanic acid, so that the conductivity and the lithium ion migration rate of the prepared doped lithium titanate can be effectively improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a schematic microstructure of a first embodiment of a doped lithium titanate according to the invention;
fig. 2 shows a schematic microstructure of a second embodiment of a doped lithium titanate according to the invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those illustrated or otherwise described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
Exemplary embodiments according to the present application will now be described in more detail with reference to the accompanying drawings. These exemplary embodiments may, however, be embodied in many different forms and should not be construed as limited to only the embodiments set forth herein. It is to be understood that these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the exemplary embodiments to those skilled in the art, in the drawings, it is possible to enlarge the thicknesses of layers and regions for clarity, and the same devices are denoted by the same reference numerals, and thus the description thereof will be omitted.
Referring to fig. 1 to 2, according to an embodiment of the present application, a method for preparing doped lithium titanate is provided.
Specifically, the method for doping lithium titanate comprises the following steps: using a mixed solution of polyethylene glycol and water as a hydrolysis solvent of titanyl sulfate; adding titanyl sulfate into a hydrolysis solvent, adding a compound containing metal ions into the hydrolysis solvent, and allowing the metal ions in the compound containing metal ions to participate in the hydrolysis reaction of the titanyl sulfate to obtain a precursor comprising doped metatitanic acid and polyethylene glycol; and mixing the precursor with a lithium source, and carrying out chemical reaction on the precursor and the lithium source to obtain the doped lithium titanate.
By applying the technical scheme of the invention, the mixed solution of polyethylene glycol and water is used as a hydrolysis solvent of titanyl sulfate, and the polyethylene glycol can prevent excessive agglomeration of doped metatitanic acid generated after hydrolysis of titanyl sulfate, so that the prepared doped lithium titanate has smaller primary particles, and further the ion migration path of the doped lithium titanate is shorter, and the lithium ion migration rate is higher; polyethylene glycol is contained in the doped lithium titanate as a carbon source, so that the conductivity of the doped lithium titanate is improved. Meanwhile, a compound of specific metal ions is added into a hydrolysis solvent, so that the metal ions participate in titanyl sulfate hydrolysis reaction, and the metal ions are uniformly doped into the doped metatitanic acid, so that the conductivity and the lithium ion migration rate of the prepared doped lithium titanate can be effectively improved.
Preferably, according to the technical scheme, a doped metatitanic acid and polyethylene glycol precursor is prepared, and then the precursor and a lithium source are mixed to prepare the lithium titanate negative electrode material. The preparation process of the precursor is as follows: the mixed solvent of polyethylene glycol and water is used as a hydrolysis solvent of titanyl sulfate, a doped metal reagent is added in a hydrolysis link to obtain doped metatitanic acid doped with metal elements with low agglomeration degree, and then the mixed solvent of polyethylene glycol and water is used for washing the doped metatitanic acid to obtain the doped metatitanic acid containing polyethylene glycol. And (3) carrying out spray drying on the doped metatitanic acid containing polyethylene glycol to obtain a precursor of the doped metatitanic acid and the polyethylene glycol. The precursor and the lithium source are mixed and sintered in an inert atmosphere to obtain doped lithium titanate, and the lithium battery prepared by using the doped lithium titanate as a negative electrode material has excellent performance under the condition of high-rate charge and discharge.
It should be noted that metatitanic acid required for the doped process flow can be purchased from the market, or can be refined from ilmenite. The method comprises the steps of firstly, grinding raw ore, namely grinding the raw ore to the fineness required by the process, generally about 325 meshes, carrying out acidolysis on the raw ore powder, preferably adding 65-75% of sulfuric acid by mass into a sulfuric acid solution at the temperature of 150-160 ℃, obtaining a titanium solution with higher concentration, and then adding a proper amount of ammonia water into the titanium solution to promote hydrolysis of titanyl sulfate so as to obtain metatitanic acid.
Further, the compound containing the metal ions is one or more of an oxide of the metal M, a hydroxide of the metal M, a sulfate of the metal M and a sulfate oxide of the metal M, wherein M is one or a combination of more of Ag, Au, Cu, Zr, Mg, Nb, Ca, V, Sr and Mo. The metal ions in the compound containing the metal ions participate in the hydrolysis reaction of the titanyl sulfate, and the obtained product is the doped metatitanic acid doped with the metal ions. The doping of the compound containing metal ions is realized in the hydrolysis link of titanyl sulfate in the process of preparing titanium dioxide sulfate by a sulfuric acid method.
Specifically, the doped metatitanic acid has a structural formula of H2TixM1-xO3, wherein x is in a value range of 0.0-0.99. The doped lithium titanate produced after doping metal particles has improved conductivity or lithium ion transfer efficiency. The doped metatitanic acid is H2TixM1-xO3 formed by doping M metal into H2TiO3 crystal lattice.
The mass ratio of the polyethylene glycol to the water in the mixed solution of the polyethylene glycol and the water is 9: 1-1: 9. The content of carbon element in the doped lithium titanate can be indirectly adjusted by adjusting the mass ratio of the polyethylene glycol to the water in the mixed solution of the polyethylene glycol and the water, so that the composite performance of the doped lithium titanate is controlled. Polyethylene glycol and water are used as a mixed solvent, the polyethylene glycol can be used as an anti-agglomeration agent to reduce the particle size of the doped metatitanic acid material, and can also be used as a carbon source in the synthesis reaction of the doped lithium titanate material, so that the synergistic improvement of the rate capability is realized. The mass ratio of polyethylene glycol to water in the mixed solution of polyethylene glycol and water is 9: 1-1: 9, so that doped metatitanic acid with low polymerization degree is obtained, and the mixed solvent of polyethylene glycol and water is continuously used for washing the doped metatitanic acid, so that a pure doped metatitanic acid wet material is obtained.
Furthermore, the physical diameter of the primary particle of the doped lithium titanate is between 100 and 400 nm. As shown in fig. 1, a Scanning Electron Microscope (SEM) image of the synthesized doped lithium titanate material magnified 20000 times, and it can be seen in fig. 1 that the physical diameter of primary particles of the doped lithium titanate is small and the pores between the primary particles are small. Fig. 2 is a Scanning Electron Microscope (SEM) image of 10000 times magnification of the material of the doped metatitanic acid, which shows that the overall better sphericity of the doped metatitanic acid is obtained.
Further, the step of chemically reacting the precursor and the lithium source comprises: and mixing the precursor and a lithium source, ball-milling, and sintering the obtained solid mixture at 730-750 ℃ in an inert atmosphere to obtain the doped lithium titanate. Preferably, the solid mixture of the precursor and the lithium source is sintered at 740 ℃ under an inert atmosphere to obtain the doped lithium titanate. The solid-phase method is adopted to synthesize the lithium titanate, the calcining temperature of the solid mixture has larger influence on the cycle performance of the lithium titanate, and the doped metatitanic acid has higher activity, so the synthesis reaction temperature for synthesizing the doped lithium titanate by the solid-phase method is lower, and the energy consumption is also lower.
Further, after the step of hydrolyzing, the method further comprises: and washing a product obtained by the hydrolysis reaction by using a mixed solution of polyethylene glycol and water, and then filtering and drying to obtain a precursor. The product obtained by the hydrolysis reaction is washed by using a mixed solution of polyethylene glycol and water, so that ferrous ions and other impurities in the hydrolyzed product can be removed.
Further, after the hydrolysis reaction step and before the washing step, the method further comprises: heating the reaction slurry obtained by the hydrolysis reaction to 60-80 ℃, adding ammonia water for neutralization, controlling the pH value of a neutralization end point to be 6.0-7.0, uniformly stirring, curing for 0.5-2 h, collecting the cured product, and washing; the drying process adopts a spray drying mode.
According to another aspect of the present invention, there is provided a doped lithium titanate prepared by the above method.
According to another aspect of the invention, a lithium ion battery negative electrode material is provided, and comprises the doped lithium titanate. The lithium ion battery prepared by adopting the doped lithium titanate as the cathode material has obviously improved conductivity, shorter lithium ion migration path and excellent performance under the condition of high-rate charge and discharge.
The technical scheme of the application provides the doped metatitanic acid for synthesizing the doped lithium titanate material, and polyethylene glycol used in the process of preparing the doped metatitanic acid can effectively reduce the agglomeration degree of hydrolyzed metatitanic acid, so that the physical size of primary particles of the synthesized doped lithium titanate material is smaller.
By applying the technical scheme of the invention, polyethylene glycol and water are used as a mixed solvent in the preparation process of the titanium source, so that the agglomeration degree of the hydrolyzed doped metatitanic acid can be reduced, meanwhile, the polyethylene glycol combined with the doped metatitanic acid can also be used as a carbon source to be compounded into the doped lithium titanate material, the physical size of primary particles of the doped lithium titanate material is reduced, the added carbon source improves the conductivity of the material, and the unification of shortening a lithium ion migration path and improving the conductivity of the material is realized.
In one exemplary embodiment, a doping agent for Zr is added in the titanyl sulfate hydrolysis stage, the Zr added being in the form of Zr (SO)4)2. In the hydrolysis link, the mass concentration of titanium in hydrolysate is 200g/L, the mass ratio of polyethylene glycol to water in the hydrolysate is 1:5, the boiling state during hydrolysis is explosive boiling, the hydrolysis temperature is 115 ℃, the molar ratio of acid titanium (the ratio of hydrogen ions to titanium ions in the hydrolysate) is 1.8, the hydrolysis time is 4 hours, the hydrolyzed metatitanic acid slurry is taken, the metatitanic acid slurry obtained through hydrolysis reaction is heated to 60-80 ℃, ammonia water is added for neutralization, the end point pH value is controlled to be 6.0-7.0, the mixture is uniformly stirred and cured for 0.5-2 hours, then the mixture is washed with mixed solvent of polyethylene glycol and water for 15-40 minutes, wet metatitanic acid slurry is obtained after filtration, and the wet metatitanic acid slurry is sprayedAnd (4) carrying out spray drying to obtain a doped metatitanic acid and polyethylene glycol precursor. In this example, the chemical formula of the obtained doped metatitanic acid is H2Ti0.99Zr0.01O3。
Specifically, the synthesis method of the doped lithium titanate comprises the steps of directly mixing the precursor and a lithium source, fully and uniformly mixing the materials in a ball milling mode, and sintering the obtained solid mixture at 740 ℃ in an inert atmosphere to complete the preparation of the doped lithium titanate material.
Further, the doped lithium titanate material was tested: with 1mol/L LiPF6 conductive salt and DMC DEC: EC (wt%) ═ 1: 1: 1 as an electrolyte. Under the charging and discharging conditions of 1C/1C and 1.3-2.4v, the discharge capacity of the doped lithium titanate material is 170.5mAh/g, and the primary efficiency is 99.37%. The following table shows a ratio comparison table when the charge/discharge ratio of the material of the present example is 1C to 10C.
Figure BDA0003255383330000051
Spatially relative terms, such as "above … …," "above … …," "above … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial relationship to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary term "above … …" can include both an orientation of "above … …" and "below … …". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
In addition to the foregoing, it should be noted that reference throughout this specification to "one embodiment," "another embodiment," "an embodiment," or the like, means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment described generally throughout this application. The appearances of the same phrase in various places in the specification are not necessarily all referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with any embodiment, it is submitted that it is within the scope of the invention to effect such feature, structure, or characteristic in connection with other embodiments.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A method of preparing doped lithium titanate, comprising:
using a mixed solution of polyethylene glycol and water as a hydrolysis solvent of titanyl sulfate;
adding titanyl sulfate into the hydrolysis solvent, adding a compound containing metal ions into the hydrolysis solvent, and allowing the metal ions in the compound containing metal ions to participate in the hydrolysis reaction of the titanyl sulfate to obtain a precursor containing doped metatitanic acid and polyethylene glycol;
and mixing the precursor with a lithium source, and carrying out chemical reaction on the precursor and the lithium source to obtain the doped lithium titanate.
2. The method according to claim 1, wherein the compound containing metal ions is one or more of an oxide of metal M, a hydroxide of metal M, a sulfate of metal M, and a sulfate oxide of metal M, wherein M is one or more of Ag, Au, Cu, Zr, Mg, Nb, Ca, V, Sr, and Mo.
3. The method of claim 2, wherein the doped metatitanic acid is of formula H2TixM1-xO3Wherein the value range of x is 0.0-0.99.
4. The method according to any one of claims 1 to 3, wherein the mass ratio of the polyethylene glycol to the water in the mixed solution of the polyethylene glycol and the water is 9: 1-1: 9.
5. The method according to any one of claims 1 to 3, wherein the primary particle physical diameter of the doped lithium titanate is between 100 and 400 nm.
6. The method of any one of claims 1 to 3, wherein the step of chemically reacting the precursor and the lithium source comprises: and mixing and ball-milling the precursor and the lithium source, and sintering the obtained solid mixture at 730-750 ℃ in an inert atmosphere to obtain the doped lithium titanate.
7. The method according to any one of claims 1 to 3, wherein after the step of hydrolysis reaction, the method further comprises: and washing a product obtained by the hydrolysis reaction by using the mixed solution of the polyethylene glycol and water, and then filtering and drying to obtain the precursor.
8. The method of claim 7, wherein after the step of hydrolysis reaction and before the step of washing, the method further comprises: heating the reaction slurry obtained by the hydrolysis reaction to 60-80 ℃, adding ammonia water for neutralization, controlling the pH value of a neutralization end point to be 6.0-7.0, uniformly stirring, curing for 0.5-2 h, collecting a cured product, and performing the washing step; the drying process adopts a spray drying mode.
9. Doped lithium titanate, characterized in that it is obtained by a process according to any one of claims 1 to 8.
10. A negative electrode material for a lithium ion battery, comprising the doped lithium titanate according to claim 9.
CN202111058178.8A 2021-09-09 2021-09-09 Method for preparing doped lithium titanate, doped lithium titanate and lithium ion battery cathode material with doped lithium titanate Pending CN113921811A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117117157A (en) * 2023-10-23 2023-11-24 北京科技大学 Lithium ion battery negative electrode material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117117157A (en) * 2023-10-23 2023-11-24 北京科技大学 Lithium ion battery negative electrode material and preparation method thereof
CN117117157B (en) * 2023-10-23 2024-01-23 北京科技大学 Lithium ion battery negative electrode material and preparation method thereof

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