CN112331854A - Lithium magnesium silicate pre-lithiated silicon monoxide negative electrode material and preparation method and application thereof - Google Patents
Lithium magnesium silicate pre-lithiated silicon monoxide negative electrode material and preparation method and application thereof Download PDFInfo
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- 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
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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
- 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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a magnesium lithium silicate pre-lithiation silicon monoxide negative electrode material, which comprises the following steps: (1) preparing materials: obtaining a silicon monoxide negative powder, wherein the silicon monoxide negative powder is a silicon monoxide powder which is not subjected to disproportionation treatment; obtaining lithium oxide powder, wherein the lithium oxide powder is analytically pure and anhydrous lithium oxide powder; obtaining magnesium oxide powder, wherein the magnesium oxide powder is analytically pure, (2) mixing: adding the silicon monoxide powder, the lithium oxide powder and the magnesium oxide powder into a mixer according to a certain proportion, and stirring and mixing at normal temperature to obtain uniform mixed powder A; (3) and (3) heat treatment: carrying out heat treatment reaction on the mixed powder A in the step (2) under inert gas to obtain an intermediate product B; (4) CVD carbon coating: and (3) performing carbon coating on the intermediate product B obtained in the step (3) under a carbon source gas by using a chemical vapor deposition method, wherein the prepared product has high first coulombic efficiency and good cycle stability.
Description
Technical Field
The invention relates to the technical field of battery cathode materials, in particular to a magnesium lithium silicate pre-lithiation silicon monoxide cathode material and a preparation method and application thereof.
Background
Currently, Lithium Ion Batteries (LIBs) are widely used in the field of power energy, and silicon-based materials have extremely high lithium storage capacity and are considered as the most promising materials for replacing graphite cathodes or other carbon cathodes. But the silicon-based negative electrode can cause larger volume expansion in the lithium-intercalation and deintercalation process, and simultaneously an SEI film is easy to form for repeated growth, so that a large amount of active lithium is lost in the first charge-discharge cycle, irreversible capacity is caused, and the cycle performance is poor. In a silicon-based material, the SiO has small volume expansion and the theoretical capacity of 1200mA h g−1The lithium ion battery cathode material has good cyclicity, is a hot spot of the current commercial research of the lithium ion battery cathode material, has low Initial Coulombic Efficiency (ICE) due to irreversible consumption of partial active lithium in the initial cycle process, limits the commercial popularization of SiO, carries out pre-lithiation treatment on the cathode material, and carries out non-crystalline silicon dioxide (SiO) in silicon monoxide2) The lithium silicate in a stable phase is consumed in advance and fully reacted, and the first coulombic efficiency is improved.
Master thesis 'study on modification of lithium titanate serving as a lithium battery negative electrode material and a capacity fading mechanism thereof' in chapter five, LTO is modified by magnesium lithium silicate, the magnesium lithium silicate and the LTO are mixed in an aqueous solution system and sintered for 5 hours at 700 ℃, and magnesium and silicon in the magnesium lithium silicate are doped to improve the electronic conductivity and cation exchange capacity, so that the lithium ion transfer efficiency is improved. The application of the magnesium lithium silicate in other cathodes is quite wide, and the magnesium lithium silicate is used for pre-lithiating the silicon monoxide cathode, so that the first coulombic efficiency can be improved, and the conductivity of the silicon monoxide and the transmission efficiency of lithium ions can also be improved.
Disclosure of Invention
The invention aims to provide a magnesium lithium silicate prelithiation silicon monoxide negative electrode material, a preparation method and application thereof, and the prepared product has higher first coulombic efficiency and good cycling stability.
In order to achieve the above object, in a first aspect, the invention provides a method for preparing a magnesium lithium silicate prelithiation silicon monoxide negative electrode material, which comprises the following steps:
(1) preparing materials: obtaining a silicon monoxide negative powder, wherein the silicon monoxide negative powder is a silicon monoxide powder which is not subjected to disproportionation treatment; obtaining lithium oxide powder, wherein the lithium oxide powder is analytically pure and anhydrous lithium oxide powder; obtaining magnesium oxide powder, wherein the magnesium oxide powder is analytically pure;
(2) mixing materials: adding the silicon monoxide powder, the lithium oxide powder and the magnesium oxide powder into a mixer according to a certain proportion, and stirring and mixing at normal temperature to obtain uniform mixed powder A;
(3) and (3) heat treatment: carrying out heat treatment reaction on the mixed powder A in the step (2) under inert gas to obtain an intermediate product B;
(4) CVD carbon coating: and (4) carrying out carbon coating on the intermediate product B obtained in the step (3) under a carbon source gas by a chemical vapor deposition method to prepare the magnesium lithium silicate pre-lithiation silicon oxide negative electrode material.
Further, in the step (1), the silica powder is commercial silica powder and has a particle diameter d50Is 0.1-10 μm.
Further, in the step (2), the ratio of the silica powder: magnesium oxide powder: the molar ratio of the lithium oxide powder is 2: 2:1-10: 2:1.
Further, in the step (2), the mixing rotation speed of the mixer is 200-300 rpm/min, and the mixing time is 2 hours.
Further, in the step (3), the temperature of the heat treatment reaction is 1000-1300 ℃, and the reaction time is 3-8 hours.
Further, in the step (3), the inert gas is one or a mixture of several of nitrogen, helium, neon, argon, krypton, xenon and radon, wherein the aeration rate of the inert gas is 100-.
Further, in the step (4), the carbon source gas is one or a mixture of several of methane, ethane, propane, ethylene, propylene and acetylene.
Further, in the step (4), the coating temperature of the carbon coating is 650-850 ℃, and the coating time is 1-3 hours.
In a second aspect, the invention provides a magnesium lithium silicate prelithiated silicon oxide negative electrode material prepared by the preparation method as described in any one of the above technical solutions.
In a third aspect, the invention provides an application of the magnesium lithium silicate prelithiation silicon monoxide negative electrode material as described in the above technical scheme as a negative electrode material of a lithium ion battery.
In summary, the technical scheme of the preparation method of the magnesium lithium silicate pre-lithiation silicon monoxide negative electrode material at least has the following beneficial effects: the preparation method of the lithium magnesium silicate pre-lithiation silicon monoxide negative electrode material comprises the steps of taking silicon monoxide as a battery negative electrode material, and carrying out high-temperature heat treatment in advance by virtue of mixing lithium oxide and magnesium oxide to ensure that amorphous silicon dioxide in the silicon monoxide is consumed in advance and fully reacts to generate stable-phase lithium silicate to form SiO/Si/LixMgyOzSinThe irreversible stable phase is formed in advance, so that the negative electrode material has high initial coulombic efficiency in the effective active lithium extraction and insertion process in the initial charge-discharge cycle process of the half-cell, and in addition, the magnesium lithium silicate has a relatively low pH value (7-9), has cation exchange property and a three-dimensional ion diffusion channel, is convenient for the lithium ion to be inserted and extracted, and obtains high electronic and ionic conductivity after the negative electrode material is modified.
In order to make the present invention and other objects, advantages, features and functions more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is an SEM picture of commercial silica;
FIG. 2 is an XRD pattern of the final product-1 (b) prepared by the steps of example 1;
FIG. 3 is an SEM picture of intermediate B-1 prepared in example 1;
FIG. 4 is an SEM photograph of the final product-1 prepared in example 1;
fig. 5 is an XRD picture (a) of the final product-2 prepared in comparative example 1 and an XRD picture (b) of the final product-3 prepared in comparative example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This embodiment 1 provides a method for preparing a magnesium lithium silicate pre-lithiated silicon monoxide negative electrode material, which specifically includes the following steps:
(1) putting a certain amount of commercial silicon monoxide powder, magnesium oxide powder and lithium oxide powder into a mixer according to the molar ratio of 5:2:1, wherein the rotating speed of the mixer is 200rpm/min, and the mixing time is 2 hours, so that powder A with uniform components is obtained;
(2) 10g of the powder A obtained in the step (1) is placed in a corundum-mullite crucible for heat treatment, high-purity argon is introduced in the atmosphere, the duration time is the whole temperature rising process and the whole temperature reduction process, the temperature rising rate is 5 ℃/min, the heat treatment temperature is 1200 ℃, the heat preservation time is 5 hours, and an intermediate product B-1 is obtained after calcination;
(3) carrying out CVD carbon coating on the intermediate product B prepared in the step (2), placing a sample in a corundum-mullite crucible, and introducing an atmosphere C2H2Gas, temperature rate of 5 ℃/min, CVDThe temperature is 750 ℃, the time is 2 hours, and the lithium magnesium silicate is taken out after natural cooling, so as to obtain the lithium magnesium silicate pre-lithiation silicon oxide negative electrode material.
Example 2
The preparation process of this example 2 is identical to that of example 1, except that the molar ratio of the silica powder, the magnesium oxide powder and the lithium oxide powder in step (1) is 4:2: 1.
The product morphology was similar to the final product prepared in example 1 as tested.
Example 3
The manufacturing process of this example 3 is exactly the same as that of example 1, except that the molar ratio of the silica powder, the magnesium oxide powder and the lithium oxide powder in step (1) is 6:2: 1.
The product morphology was similar to the final product prepared in example 1 as tested.
Example 4
The manufacturing process of this example 4 is identical to that of example 1 except that the heat treatment temperature in step (2) is replaced with 1250 ℃.
The product morphology was similar to the final product prepared in example 1 as tested.
Example 5
The manufacturing process of this example 5 is exactly the same as that of example 1 except that the heat treatment temperature in step (2) is replaced with 1300 ℃.
The product morphology was similar to the final product prepared in example 1 as tested.
FIG. 1 shows SEM pictures of commercial silica, and it can be seen from the observation of FIG. 1 that the size of commercial silica is between 2-10 μm and the surface is smooth.
FIG. 2 shows an XRD pattern of a final product-1 obtained in example 1, and from the observation of FIG. 2, it can be seen that Si, Li-containing particles were formed after the calcination treatment by mixing with lithium carbonate powder2SiO3，LixMgySizOnThe multiphase material of (1).
FIG. 3 shows an SEM picture of intermediate product B-1 prepared in step (2) of example 1. when observing FIG. 3, intermediate product B-1 is consistent with commercial silica in size ranging from 2 to 10 μm, and a slightly wrinkled layer is formed on the surface.
Fig. 4 shows an SEM picture of the final product-1 prepared in step (3) of example 1, and it can be seen from the observation of fig. 4 that the size of the final product-1 is not significantly changed compared to the intermediate product B-1, but the coating of the carbon layer is significantly observed.
Comparative example 1
The production process of this comparative example 1 was exactly the same as in example 1 except that all of the three powders taken in step (1) were replaced with lithium carbonate, that is, powder a was replaced with lithium carbonate powder.
FIG. 5 (a) is an XRD pattern of intermediate product B-2 obtained in the present comparative example 1, and it can be seen that the product is not produced with lithium magnesium silicate.
Comparative example 2
The production process of this comparative example 2 is exactly the same as in example 1 except that all of the three powders taken in step (1) are replaced with lithium oxide powder, that is, powder a is replaced with lithium oxide powder.
FIG. 5 (B) is an XRD pattern of intermediate product B-3 obtained in the present comparative example 2, and it can be seen that the product is not produced with lithium magnesium silicate.
Application example
In the preparation of all pole pieces, carbon black (SP) is used as a conductive agent, sodium carboxymethyl cellulose (CMC) is used as a binder, and the mass ratio of the conductive agent to the synthesized active material is 2: 2: 6, mixing and dissolving the mixture in deionized water and a small amount of alcohol, and magnetically stirring for more than 8 hours to prepare uniformly dispersed battery slurry for later use. The battery slurry is uniformly coated on the surface of an electrode (cut foam copper or copper foil), vacuum-dried at 85 ℃ for 12 hours, pressed into tablets and weighed for later use. The electrochemical performance of the electrodes was tested by assembling a button-type half cell (CR 2032) using a glove box (model Mbraun) from Labstar, Germany. The button half cell assembly completely adopts a lithium sheet as a counter electrode, a foam nickel sheet as a buffer gasket, and the water oxygen content of the manufacturing environment is respectively as follows: water concentration < 0.5 ppm, oxygen concentration < 1 ppm. The electrolyte used was 1M LiPF6 dissolved in EC and DMC organic solvents. Cell cycle formation was tested on novice devices.
Comparative example SiO @ C was obtained directly from a silicon monoxide coated by decomposition of carbon by CVD.
The first coulombic efficiencies of the anode materials prepared in examples 1 to 5, comparative examples 1 to 2 and comparative example SiO @ C were measured, and the measurement data are shown in table 1 below.
TABLE 1
As can be seen from the data in table 1, examples 1 to 5 are improved in both charge and discharge capacity and first coulombic efficiency as compared to comparative examples 1 to 2, and are improved in first coulombic efficiency as compared to comparative example SiO @ C.
The preparation method of the magnesium lithium silicate prelithiation silicon monoxide negative electrode material comprises the steps of taking silicon monoxide as a battery negative electrode material, and carrying out high-temperature heat treatment in advance by virtue of mixed magnesium oxide and lithium carbonate to ensure that amorphous silicon dioxide in the silicon monoxide is consumed in advance and fully reacts to generate stable-phase magnesium lithium silicate to form SiO/Si/LixMgySizOnThe complex, due to the pre-formation of the irreversible stable phase, enables the negative electrode material to have higher first coulombic efficiency in the effective active lithium extraction and insertion process during the first charge-discharge cycle of the half-cell.
The preparation method has low manufacturing cost, does not need to use liquid phase materials and equipment, has simple and controllable process, does not generate toxic substances in the preparation process, does not need to remove redundant metal chemicals in the product, and is beneficial to industrial large-scale production.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a magnesium lithium silicate pre-lithiated silicon monoxide negative electrode material is characterized by comprising the following steps:
(1) preparing materials: obtaining a silicon monoxide negative powder, wherein the silicon monoxide negative powder is a silicon monoxide powder which is not subjected to disproportionation treatment; obtaining lithium oxide powder, wherein the lithium oxide powder is analytically pure and anhydrous lithium oxide powder; obtaining magnesium oxide powder, wherein the magnesium oxide powder is analytically pure;
(2) mixing materials: adding the silicon monoxide powder, the lithium oxide powder and the magnesium oxide powder into a mixer according to a certain proportion, and stirring and mixing at normal temperature to obtain uniform mixed powder A;
(3) and (3) heat treatment: carrying out heat treatment reaction on the mixed powder A in the step (2) under inert gas to obtain an intermediate product B;
(4) CVD carbon coating: and (3) carrying out carbon coating on the intermediate product B obtained in the step (3) under a carbon source gas by a chemical vapor deposition method to prepare the pre-lithiated silicon oxide negative electrode material.
2. The method for preparing the lithium magnesium silicate prelithiation silicon monoxide negative electrode material as claimed in claim 1, wherein in step (1), the silicon monoxide powder is commercial silicon monoxide powder, and the particle diameter d50Is 0.1-10 μm.
3. The method for preparing the lithium magnesium silicate prelithiated silicon monoxide negative electrode material according to claim 1, wherein in the step (2), the silicon monoxide powder: magnesium oxide powder: the molar ratio of the lithium oxide powder is 2: 2:1-10: 2:1.
4. The method for preparing the lithium magnesium silicate prelithiation silicon monoxide negative electrode material as claimed in claim 1, wherein in the step (2), the mixing speed of the mixer is 200-300 rpm/min, and the mixing time is 2 hours.
5. The method for preparing a lithium magnesium silicate prelithiated silicon monoxide negative electrode material as recited in claim 1, wherein in step (3), the temperature of the heat treatment reaction is 1000-1300 ℃, and the reaction time is 3-8 hours.
6. The method for preparing the lithium magnesium silicate prelithiated silicon monoxide negative electrode material as claimed in claim 1, wherein in step (3), the inert gas is one or more of nitrogen, helium, neon, argon, krypton, xenon, and radon, and the aeration rate of the inert gas is 100-200 mL/h.
7. The method for preparing the lithium magnesium silicate prelithiated silicon monoxide negative electrode material according to claim 1, wherein in the step (4), the carbon source gas is one or a mixture of methane, ethane, propane, ethylene, propylene and acetylene.
8. The method for preparing the lithium magnesium silicate prelithiation silicon monoxide negative electrode material as claimed in claim 1, wherein in the step (4), the coating temperature of the carbon coating is 650-850 ℃, and the coating time is 1-3 hours.
9. A lithium magnesium silicate prelithiated silicon oxide negative electrode material prepared by the preparation method as claimed in any one of claims 1 to 8.
10. Use of the lithium magnesium silicate prelithiated silicon oxide negative electrode material of claim 9 as a negative electrode material for a lithium ion battery.
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| JP2014082118A (en) * | 2012-10-17 | 2014-05-08 | Toyota Industries Corp | Negative electrode material for lithium ion secondary battery, and negative electrode using the same, and secondary battery |
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| CN111082006A (en) * | 2019-12-06 | 2020-04-28 | 深圳市比克动力电池有限公司 | Silicon monoxide composite negative electrode material, preparation method thereof and lithium ion battery |
| CN111342030A (en) * | 2020-03-28 | 2020-06-26 | 兰溪致德新能源材料有限公司 | Multi-element composite high-first-efficiency lithium battery negative electrode material and preparation method thereof |
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- 2020-10-30 CN CN202011192354.2A patent/CN112331854A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2014082118A (en) * | 2012-10-17 | 2014-05-08 | Toyota Industries Corp | Negative electrode material for lithium ion secondary battery, and negative electrode using the same, and secondary battery |
| JP2017204374A (en) * | 2016-05-11 | 2017-11-16 | 株式会社大阪チタニウムテクノロジーズ | Silicon oxide-based powder negative electrode material |
| CN109524650A (en) * | 2018-11-13 | 2019-03-26 | 东莞市凯金新能源科技股份有限公司 | A kind of lithium ion battery silicon monoxide composite cathode material and preparation method |
| CN111082006A (en) * | 2019-12-06 | 2020-04-28 | 深圳市比克动力电池有限公司 | Silicon monoxide composite negative electrode material, preparation method thereof and lithium ion battery |
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