CN113571677A - Modification method for improving first coulombic efficiency of carbon-based negative electrode material - Google Patents

Modification method for improving first coulombic efficiency of carbon-based negative electrode material Download PDF

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CN113571677A
CN113571677A CN202110534377.5A CN202110534377A CN113571677A CN 113571677 A CN113571677 A CN 113571677A CN 202110534377 A CN202110534377 A CN 202110534377A CN 113571677 A CN113571677 A CN 113571677A
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carbon
tio
negative electrode
modification method
coulombic efficiency
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王君
毕翔宇
张稚雅
唐天宇
葛旭辉
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Lanzhou University
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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
    • H01M4/58—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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

Abstract

The invention relates to the technical field of lithium ion secondary batteries, in particular to a modification method for improving the first coulombic efficiency of a carbon-based negative electrode material, and belongs to the field of new energy materials. The method comprises the following steps: (1) taking coal as a raw material and glucose as a raw material, carrying out low-temperature heat treatment on the raw material, and (2) uniformly dispersing the carbon material prepared in the step (1), hydroxypropyl cellulose, tetrabutyl titanate and deionized water in a three-neck flask filled with ethanol according to a certain mass ratio, carrying out reaction at 90 ℃, centrifugally collecting a sample after the reaction is finished, and carrying out next-step heat treatment to obtain the negative electrode material for the lithium ion battery. The invention coats a layer of TiO on the surface of the carbon material2On the one hand, the LUMO rail of the electron-facing electrolyte is improvedAnd on the other hand, electrons are prevented from entering an electrolyte LUMO track through tunneling, so that irreversible loss of lithium ions caused by decomposition of an organic electrolyte is avoided, and the first coulomb efficiency is improved.

Description

Modification method for improving first coulombic efficiency of carbon-based negative electrode material
Technical Field
The invention belongs to the technical field of new energy, and particularly relates to a modification method for improving the first coulombic efficiency of a carbon-based material of a lithium ion battery.
Background
Lithium ion batteries are widely used in the fields of portable devices, electric vehicles, and the like due to their advantages of high operating voltage, high energy density, long cycle life, low self-discharge rate, and the like. The carbon material is a negative electrode material which is most widely applied in lithium ion batteries, however, the carbon material contacts with an organic electrolyte solution to form a solid electrolyte interface (SEI film) in the first charge and discharge process, and a large amount of lithium ions are consumed in the SEI film forming process, so that irreversible capacity loss is caused. Therefore, reducing the loss of lithium ions during the first charge and discharge process is an important problem to be solved in the field of lithium ion batteries.
The invention provides a modification method for improving the first coulombic efficiency of a carbon-based negative electrode material, aiming at the problem of low first coulombic efficiency of a carbon negative electrode. The method uses tetrabutyl titanate as a precursor, and artificially synthesized carbon nanospheres and coal-based materials as carbon sources to prepare the carbon cathode coated by anatase titanium dioxide. The method has the basic principle that a layer of titanium dioxide is coated on the surface of a carbon material, so that the transfer potential barrier of electrons to an electrolyte LUMO track is improved, the electrons are prevented from entering the electrolyte LUMO track through tunneling, the irreversible loss of lithium ions caused by decomposition of an organic electrolyte is avoided, and the first coulombic efficiency is improved.
Disclosure of Invention
(1) The principle of the invention is as follows:
in the lithium intercalation process, the electrochemical potential of the negative electrode is higher than the LUMO orbit of the electrolyte, electrons automatically enter the LUMO orbit to decompose the electrolyte, and the decomposed electrolyte forms a layer of solid electrolyte film (SEI) with a certain thickness on the surface of the negative electrode, at this time, the electrons cannot cross the potential barrier of the SEI and cannot tunnel the SEI to the LUMO orbit, so as to reach a stable state, as shown in fig. 1 (a).
The core idea of this invention is to utilize a lithium ion battery with Li+Half of storage capacityThe conductive material is formed with a coating layer with a certain thickness in advance, the coating layer can prevent the electron tunneling from reaching the LUMO orbit on one hand, on the other hand, the coating layer can increase the resistance of the electron directly entering the LUMO due to a certain potential barrier, and during the lithium intercalation process, the stable state can be reached as long as a very thin SEI layer is formed to prevent the electron from crossing the potential barrier and entering the LUMO, as shown in FIG. 1 (b).
(2) Technical scheme
The invention provides a method for improving the first coulombic efficiency of a carbon-based negative electrode material, which comprises the following raw materials: the invention relates to bituminous coal and artificially synthesized carbon microspheres, which are realized by the following technical scheme:
(1) preparation of carbon material: the carbon material for the lithium ion battery is obtained by taking bituminous coal and glucose as carbon sources and performing simple heat treatment.
(2)C@TiO2The preparation of (1): uniformly dispersing hydroxypropyl cellulose, tetrabutyl titanate, deionized water and a carbon material into an ethanol solution according to the mass ratio of 5:5:20:1, adding the prepared solution into a three-neck flask, carrying out water bath at 90 ℃ for 3 hours in a water bath kettle, centrifuging after the water bath is finished, collecting a sample, and drying in an oven. Carrying out heat treatment on the dried powder for 1h at 600 ℃ under the protection of argon to obtain TiO2A coated carbon material.
(3) Advantageous technical effects
Compared with the prior art, the invention has the following advantages:
(1) compared with the conventional method, the preparation method provided by the invention has the advantages of relatively low cost and simple preparation process, does not adopt the procedures of conventional chemical purification and the like, and reduces the pollution of the chemical purification to the environment.
(2) Compared with a carbon cathode, the composite cathode material prepared by the invention has good electrochemical performance, and the first coulombic efficiency is improved by more than 10%.
Drawings
The present invention is described in further detail below with reference to the attached drawings.
FIGS. 1(a-b) are schematic diagrams of the present invention;
FIG. 2(a-b) is CC and CC @ TiO prepared in example 12The scanning electron microscope overview picture;
FIG. 2(c-g) is a partial magnified scanning electron microscope and EDS spectrum of CC prepared in example 1;
FIG. 2(h-l) is CC @ TiO prepared in example 12The local enlarged image of the scanning electron microscope and an EDS spectrogram;
FIG. 3 shows CG and CG @ TiO prepared in example 22Scanning electron microscope images of;
FIG. 4(a-b) is CG @ TiO prepared in example 22Transmission electron microscopy and EDS spectra of;
FIG. 5(a-b) is a schematic representation of CC and CC @ TiO prepared in example 1 of the invention2And CG @ TiO prepared in example 22(ii) a Raman spectrum of;
FIGS. 6(a-d) are graphs of CC at 0.01-2V and CC @ TiO prepared in example 1 of the invention2Voltammetric curves at 0.01-2.5V and CG @ TiO prepared in example 22Voltammetric curves at 0.01-3V;
FIG. 7(a-b) is a graph of C and C @ TiO prepared according to example 1 of the present invention2At 37.2mAg-1Current Density cycling Performance plot and C @ TiO prepared in example 22At 37.2mAg-1Cycling performance plot at current density.
Detailed Description
Experimental reagent: hydroxypropyl cellulose, tetrabutyl titanate, coal powder, glucose, deionized water, and absolute ethyl alcohol (99.9 wt%).
The instrument comprises the following steps: scanning electron microscope (MIRA3 TESCAN), Raman spectrometer (HORIBA Jobin Yvon LabRAM HR800), blue cell test system (CT 2001A, Jinnuo electronics, Inc., Wuhan City), glove box (Mikauna; filling atmosphere is argon; water oxygen value <0.1 PPM).
The reagents or instruments used in the examples are not indicated by manufacturers, and are all conventional reagent products available on the market.
Example 1
A modification method for improving the first coulombic efficiency of a carbon-based negative electrode material comprises the following specific steps:
(1) CC (carbon derived from meal) preparation: into a high-energy planetary ball millAdding 50 parts of coal ash powder, setting the revolution speed of a ball mill to be 260rpm and the rotation speed to be 640rpm, ball-milling for 12 hours until the coal powder passes through a 500-mesh screen, and putting the obtained coal powder in Ar2And under the protection of gas, heating to 700 ℃ at the heating rate of 5 ℃/min, preserving the heat for 1h, and carrying out pyrolysis to obtain the carbon material.
(2)CC@TiO2The preparation of (1): uniformly dispersing hydroxypropyl cellulose, tetrabutyl titanate, deionized water and amorphous carbon into an ethanol solution according to the mass ratio of 5:5:20:1, adding the prepared solution into a three-neck flask, carrying out water bath at 90 ℃ for three hours in a water bath kettle, centrifuging after the water bath is finished, collecting a sample, and drying in an oven. Introducing argon (60sccm) into the dried powder in a tubular furnace, and performing heat treatment at 600 ℃ for 1h to obtain CC @ TiO2。
Example 2
A modification method for improving the first coulombic efficiency of a carbon-based negative electrode material comprises the following specific steps:
(1) preparation of CG (carbon derived from glucose): 3.762g of glucose is dissolved in 35ml of deionized water, and the prepared solution is stirred for 1 hour and then placed in a hydrothermal kettle. Keeping the temperature at 175 ℃ for 12h, centrifuging after finishing, collecting a sample, and drying in an oven.
(2)CG@TiO2The preparation of (1): uniformly dispersing hydroxypropyl cellulose, tetrabutyl titanate, deionized water and carbon microspheres into an ethanol solution according to the mass ratio of 5:5:20:1, adding the prepared solution into a three-neck flask, carrying out water bath at 90 ℃ for three hours in a water bath kettle, centrifuging after the water bath is finished, collecting a sample, and drying in an oven. Introducing argon (60sccm) into the dried powder in a tube furnace, and performing heat treatment at 600 ℃ for 1h to obtain CG @ TiO2。
Example 3
A modification method for improving the first coulombic efficiency of a carbon-based negative electrode material comprises the following specific steps:
(1) CC preparation: adding 40 parts of coal ash powder into a high-energy planetary ball mill, setting the revolution speed of the ball mill to 280rpm and the rotation speed to 660rpm, ball-milling for 12 hours until the coal powder passes through a 500-mesh screen, and enabling the obtained coal powder to pass through an Ar screen2Under the protection of gas, the temperature is raised at a speed of 5 ℃/minHeating to 700 ℃ and preserving the temperature for 1h, and carrying out pyrolysis to obtain the carbon material.
(2)CC@TiO2The preparation of (1): uniformly dispersing hydroxypropyl cellulose, tetrabutyl titanate, deionized water and amorphous carbon into an ethanol solution according to the mass ratio of 5.5:4.5:21:1, adding the prepared solution into a three-neck flask, carrying out water bath at 90 ℃ for 2.5 hours in a water bath kettle, centrifuging after the water bath is finished, collecting a sample, and drying in an oven. Introducing argon (60sccm) into the dried powder in a tubular furnace, and performing heat treatment at 600 ℃ for 1h to obtain CC @ TiO2。
Example 4
A modification method for improving the first coulombic efficiency of a carbon-based negative electrode material comprises the following specific steps:
(1) preparation of CG: 3.5g of glucose is dissolved in 40ml of deionized water, and the prepared solution is stirred for 1 hour and then placed in a hydrothermal kettle. Keeping the temperature at 175 ℃ for 12h, centrifuging after finishing, collecting a sample, and drying in an oven.
(2)CG@TiO2The preparation of (1): uniformly dispersing hydroxypropyl cellulose, tetrabutyl titanate, deionized water and carbon microspheres into an ethanol solution according to the mass ratio of 4.5:5.5:19:1, adding the prepared solution into a three-neck flask, carrying out water bath at 90 ℃ for 3.5 hours in a water bath kettle, centrifuging after the water bath is finished, collecting a sample, and drying in an oven. Introducing argon (60sccm) into the dried powder in a tube furnace, and performing heat treatment at 600 ℃ for 1h to obtain CG @ TiO2。
FIG. 2(a-b) is a graph of C and C @ TiO prepared by high temperature heat treatment in example 12It can be seen from the overall view of the scanning electron microscope that the average particle size of CC was about 5 μm, the irregular shape was exhibited, and TiO was used2After coating, CC @ TiO can be seen2The particle size and the surface appearance of the particles are not obviously changed;
FIG. 2(C-g) is a partially enlarged scanning electron microscope image and an EDS spectrogram of the carbon material prepared in example 1, wherein the scanning electron microscope image shows that the surface of the CC material is smooth and flat, and the EDS spectrogram shows that the carbon material prepared is mainly composed of C element and contains a small amount of O element, because the carbon material contains some oxygen-containing volatile components, and the EDS spectrogram contains a small amount of O element;
FIG. 2(h-l) is CC @ TiO prepared in example 12The scanning electron microscope local enlarged view and the EDS spectrogram show that the C surface is covered with a layer of continuous TiO2The particles can see that Ti and O elements are uniformly distributed on the surface of the carbon material by combining an EDS spectrogram, which shows that TiO2Successfully coating the surface C;
FIG. 3(a-b) shows CG and CG @ TiO prepared in example 22The particle size of the artificially synthesized carbon spheres is mainly distributed about 200nm, and TiO is shown in the scanning electron microscope image2The shape of the coated carbon sphere is not obviously changed, but the size is slightly increased, and CG @ TiO2Compared with C, the dispersibility is greatly improved;
FIG. 4(a-b) is CG @ TiO prepared in example 22High resolution TEM images showing a fully encapsulated inner particle with an outer coating thickness of about 50nm and EDS spectra. Furthermore, the EDS spectrum shows the element distribution of the composite material, in which the carbon nanoparticles are coated with TiO2Wrapping, wherein the shell layer mainly comprises Ti and O;
FIG. 5(a-b) is a schematic representation of CC and CC @ TiO prepared in example 1 of the invention2And CG @ TiO prepared in example 22From the Raman spectrum of (A), it can be clearly seen that there are two peaks in CC and CG, namely the D peak (1342 cm) corresponding to the defect of the C atomic lattice-1) And G peak (1580 cm) representing in-plane stretching vibration of sp2 hybrid of C atom-1) The IG/ID ratios for CC and CG were 0.96 and 0.25, respectively, reflecting the lower degree of graphitization of the carbon produced. CC @ TiO2And CG @ TiO2Raman spectrum of about 150cm-1(Eg)，519cm-1(B1g) and 611cm-1Anatase type TiO is observed at wave number of (Eg)2Two characteristic peaks and the G and D peaks of carbon, indicating that anatase is TiO2The main phase of the shell.
FIGS. 6(a-d) are graphs of CC at 0.01-2V and CC @ TiO prepared in example 1 of the invention2Voltammetric curves at 0.01-2.5V and CG @ TiO prepared in example 22Voltammetric curves at 0.01-3V; TiO22Effect of coatingIs obvious. For the original CC and CG, there is a large irreversible peak around 0.58V, which is clearly due to the decomposition of the electrolyte. In contrast, for CC @ TiO2And CG @ TiO2The cyclic voltammogram of (2) shows that almost no irreversible peak was observed at around 0.58V, indicating that TiO2The coating layer can effectively inhibit the decomposition of electrolyte, reduce the irreversible loss of lithium ions and improve the first coulombic efficiency.
FIG. 7(a-b) is a graph of C and C @ TiO prepared according to example 1 of the present invention2At 37.2mAg-1Current Density cycling Performance plot and C @ TiO prepared in example 22At 37.2mAg-1The cycle performance under current density is shown in the graph, in the first 10 cycles, the specific discharge capacities of CC and CC @ TiO2 are slightly reduced to 316 mAh g and 317mAh g respectively-1. After 100 cycles, the specific discharge capacities of CC and CC @ TiO2 were 291.3 and 307.6mAh g-1. The capacity retention rate of CC is 92 percent, and CG @ TiO2Of (3) indicates TiO2The coating layer can improve the circulation stability. CG is compared with CG at TiO2The first coulombic efficiency is improved by about 15 percent, and the specific discharge capacity is improved by 200mAh g-1The capacity is improved by artificially synthesized CG @ TiO2Is a nano-material, carbon is along with TiO during heat treatment2Grain boundary diffusion forms C/TiO2The interface and the interface can increase active sites for lithium ion storage, so that the capacity of the negative electrode material is greatly improved. The CG @ TiO2 can still maintain 320mAh g after being circulated for 100 times-1The reversible capacity of (a).
Table 1 shows the charge-discharge specific capacity and the first coulombic efficiency data of the negative electrode materials prepared in examples 1 and 2 of the present invention;
TABLE 1
Figure RE-GDA0003278711320000061
The invention relates to the technical field of lithium ion secondary batteries, in particular to a modification method for improving the first coulombic efficiency of a carbon-based negative electrode material, and belongs to the field of new energy materials. The method comprises the following steps: (1) using coal as raw material and glucose as raw materialPerforming low-temperature heat treatment, (2) uniformly dispersing the carbon material prepared in the step (1), hydroxypropyl cellulose, tetrabutyl titanate and deionized water in a three-neck flask filled with ethanol according to a certain mass ratio, reacting at 90 ℃, centrifuging and collecting a sample after the reaction is finished, and performing next heat treatment to obtain the negative electrode material for the lithium ion battery. The invention coats a layer of TiO on the surface of the carbon material2On one hand, the transfer potential barrier of electrons to the electrolyte LUMO track is improved, on the other hand, the electrons are prevented from entering the electrolyte LUMO track through tunneling, and the irreversible loss of lithium ions caused by decomposition of organic electrolyte is avoided, so that the first coulomb efficiency is improved.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the invention as defined by the appended claims. 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 (3)

1. A modification method for improving the first coulombic efficiency of a carbon-based negative electrode material is characterized by comprising the following steps:
(1) preparation of carbon material: taking coal as a raw material and glucose as a raw material, and carrying out low-temperature heat treatment on the coal and the glucose to obtain a carbon material for a lithium ion battery;
(2)C@TiO2the preparation of (1): uniformly dispersing hydroxypropyl cellulose, tetrabutyl titanate, deionized water and a carbon material into an ethanol solution according to the mass ratio of 4.5-5.5:4.5-5.5:19-21:1, adding the prepared solution into a three-neck flask, carrying out water bath at 90 ℃ in a water bath kettle for 2.5-3.5h, centrifugally collecting a sample after finishing the water bath, and drying the sample in an oven; the dried powder is subjected to heat treatment for 1h at the temperature of 500-700 ℃ under the protection of argon to obtain TiO2A coated carbon material.
2. The modification method for improving the first coulombic efficiency of the carbon-based negative electrode material according to claim 1, wherein the modification method comprises the following steps: the mass ratio of the hydroxypropyl cellulose to the tetrabutyl titanate to the deionized water to the carbon material is 5:5:20: 1.
3. The modification method for improving the first coulombic efficiency of the carbon-based negative electrode material according to claim 1, wherein the modification method comprises the following steps: the water bath time was 3 h.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101425580A (en) * 2007-10-29 2009-05-06 比亚迪股份有限公司 Negative electrode active substance of lithium ionic cell and preparing method thereof, negative electrode and cell
CN103094527A (en) * 2013-01-12 2013-05-08 上海大学 Method for reducing irreversible capacity loss of cathode material of lithium ion battery in initial charge
CN104001506A (en) * 2014-06-10 2014-08-27 天津大学 Alcohol photo-oxidization catalyst, and preparation method and application thereof
WO2016202162A1 (en) * 2015-06-16 2016-12-22 田东 Method for synthesizing lithium-ion negative-electrode material li4ti5o12/c
CN108448073A (en) * 2018-02-01 2018-08-24 山东理工大学 Lithium ion battery C@TiO2Composite negative pole material and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101425580A (en) * 2007-10-29 2009-05-06 比亚迪股份有限公司 Negative electrode active substance of lithium ionic cell and preparing method thereof, negative electrode and cell
CN103094527A (en) * 2013-01-12 2013-05-08 上海大学 Method for reducing irreversible capacity loss of cathode material of lithium ion battery in initial charge
CN104001506A (en) * 2014-06-10 2014-08-27 天津大学 Alcohol photo-oxidization catalyst, and preparation method and application thereof
WO2016202162A1 (en) * 2015-06-16 2016-12-22 田东 Method for synthesizing lithium-ion negative-electrode material li4ti5o12/c
CN108448073A (en) * 2018-02-01 2018-08-24 山东理工大学 Lithium ion battery C@TiO2Composite negative pole material and preparation method thereof

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