CN112038598A - Pre-lithiated silicon monoxide negative electrode material and preparation method and application thereof - Google Patents
Pre-lithiated silicon monoxide negative electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a pre-lithiated 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 carbonate powder, wherein the lithium carbonate powder is analytically pure and anhydrous lithium carbonate powder; (2) mixing materials: adding the silicon monoxide powder and the lithium carbonate powder into a mixer according to a certain proportion, and stirring and mixing 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 using a chemical deposition method to prepare the pre-lithiated silicon oxide negative electrode material. The product prepared by the preparation method has higher first coulombic efficiency and good cycle stability, and can be used as a negative electrode material of a lithium ion battery.
Description
Technical Field
The invention relates to the technical field of battery cathode materials, in particular to a pre-lithiated silicon oxide cathode material and a preparation method and application thereof.
Background
In order to understand the increasing shortage of non-renewable fossil energy and the environmental pollution caused by the combustion of the fossil energy, clean and efficient renewable energy sources (such as wind energy, solar energy, nuclear energy and the like) become novel energy storage technologies with a prospect. Lithium Ion Batteries (LIBs) have been widely used in various electronic products nowadays, and show great application potential in the fields of electric vehicles and power grid energy storage.
The graphite cathode commonly used at present is limited by the lower theoretical capacity (372 mA h g)−1) It is difficult to meet the increasing demand for high capacity. Silicon (Si) is due to its low potential, low cost and extremely high lithium storage capacity (4200 mA h g)−1) Are considered to be the most promising materials for replacing graphite anodes or other carbon anodes. However, during the lithium intercalation/deintercalation process, the formation of lithium-silicon alloy causes a large volume expansion (300%) of the silicon negative electrode while forming a solid electrolyte interface film (SEI) and the SEI repeatedly grows during the subsequent several cycles, and active lithium is largely lost in the first cycle, resulting in irreversible capacity and poor cycle performance. Therefore, silicon-based anode materials such as silicon monoxide (SiO) are widely concerned, and compared with the huge volume change of pure silicon in the lithiation process, the SiO has smaller volume expansion and the theoretical capacity of 2400mA h g−1While maintaining good cyclability. However, there are some problems in the commercial application of SiO, one is that the intrinsic conductivity is low, decreasing the electrochemical activity of the electrode; secondly, the first coulombic efficiency (ICE) is low because the oxygen component in the SiO irreversibly consumes a part of the active lithium during the first cycle, and the lithium carbonate decomposition product lithium oxide will oxidize the amorphous silica (Si) in the silicaO2) Consumed in advance and fully reacted to form stable phase lithium silicate.
Disclosure of Invention
The invention aims to provide a pre-lithiated silicon monoxide negative electrode material and a preparation method and application thereof, and the prepared product has high first coulombic efficiency and good cycle stability.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a method for preparing a pre-lithiated silicon oxide negative electrode material, including the steps of:
(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 carbonate powder, wherein the lithium carbonate powder is analytically pure and anhydrous lithium carbonate powder;
(2) mixing materials: adding the silicon monoxide powder and the lithium carbonate powder into a mixer according to a certain proportion, and stirring and mixing 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 using a chemical deposition method to prepare the pre-lithiated 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 silicon monoxide powder to the lithium carbonate powder is 2: 1-8: 1.
Further, in the step (2), the mixing speed of the mixer is 200 rpm/min, and the mixing time is 2 hours.
Further, in the step (3), the temperature of the heat treatment reaction is 600-1100 ℃, and the reaction time is 3-7 hours.
Further, in the step (3), the inert gas is one or a mixture of nitrogen, argon and helium, wherein the aeration rate of the inert gas is 100-200 mL/min.
Further, in the step (4), the carbon source gas is one or a mixture of acetylene, ethylene, methane and ethane.
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 present invention provides a pre-lithiated silicon oxide negative electrode material prepared by the preparation method as described in any one of the above embodiments.
In a third aspect, the present invention provides the use of the prelithiated silicon oxide negative electrode material as described in the above technical solution as a negative electrode material for a lithium ion battery.
In summary, the technical scheme of the preparation method of the pre-lithiated silicon oxide negative electrode material at least has the following beneficial effects: the preparation method of the pre-lithiation silicon monoxide negative electrode material comprises the steps of taking silicon monoxide as a battery negative electrode material, carrying out high-temperature heat treatment in advance by virtue of mixed lithium carbonate, consuming amorphous silicon dioxide in the silicon monoxide in advance and fully reacting to generate stable-phase lithium silicate to form SiO/Si/LixSiyOzThe 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.
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 intermediate product B-1 (a) and 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 SEM 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 pre-lithiated silicon oxide negative electrode material, which specifically includes the following steps:
(1) taking a certain amount of commercial silicon monoxide powder and lithium carbonate powder, putting the commercial silicon monoxide powder and the lithium carbonate powder into a mixer according to the molar ratio of 5:1, wherein the mixer rotates at 200rpm for 2 hours, and mixing the silicon monoxide powder and the lithium carbonate powder to obtain powder A with uniform components;
(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 800 ℃, 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-1 prepared in the step (2), placing a sample in a corundum-mullite crucible, and introducing an atmosphere C2H2Gas, the heating rate is 5 ℃/min, the CVD temperature is 750 ℃ and the time isAnd 2 hours, obtaining a final product-1, namely the pre-lithiated silicon oxide negative electrode material.
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 XRD patterns of intermediate product B-1 (a) and final product-1 (B) obtained in example 1. from an examination of FIG. 2, it can be seen that SiO, Si and Li were formed after calcination treatment by mixing with lithium carbonate powder2SiO3And Li4SiO4The composition of the sample after CVD carbon coating is not changed.
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 manufacturing process of this comparative example 1 is exactly the same as that of example 1 except that the temperature of the heat treatment in step (2) is replaced with 500 c to obtain intermediate product B-2, final product-2.
FIG. 5 (a) is an XRD pattern of intermediate product B-2 and final product-2 obtained in the present comparative example 1, and it can be seen that no Si is generated from the products.
Comparative example 2
The manufacturing process of this comparative example 2 is exactly the same as that of example 1 except that the temperature of the heat treatment in step (2) is changed to 1200 c to obtain intermediate product B-3 and final product-3.
FIG. 5 (B) is an SEM photograph of intermediate product B-3 and final product-3 obtained in comparative example 2, and it can be seen that the surface of the products was cracked.
Example 2
The preparation process of this example 2 was exactly the same as in example 1 except that the ratio of the silicon oxide to the lithium carbonate in step (1) was 2: 1.
The product morphology was similar to the final product prepared in example 1 as tested.
Example 3
The preparation process of this example 3 was exactly the same as in example 1 except that the ratio of silica to lithium carbonate in step (1) was 8: 1.
The product morphology was similar to the final product prepared in example 1 as tested.
Example 4
The preparation process of this example 4 was identical to that of example 1 except that the heat treatment temperature in step (2) was replaced with 600 ℃.
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 1100 ℃.
The product morphology was similar to the final product prepared in example 1 as tested.
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 adopted electrolyte component is 1M LiPF6Dissolved 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 with comparative examples 1 to 2, and are improved in first coulombic efficiency as compared with comparative example SiO @ C.
The preparation method of the pre-lithiation silicon monoxide negative electrode material comprises the steps of taking silicon monoxide as a battery negative electrode material, carrying out high-temperature heat treatment in advance by virtue of mixed lithium carbonate, consuming amorphous silicon dioxide in the silicon monoxide in advance and fully reacting to generate stable-phase lithium silicate to form SiO/Si/LixSiyOzThe 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 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 carbonate powder, wherein the lithium carbonate powder is analytically pure and anhydrous lithium carbonate powder;
(2) mixing materials: adding the silicon monoxide powder and the lithium carbonate powder into a mixer according to a certain proportion, and stirring and mixing 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 using a chemical deposition method to prepare the pre-lithiated silicon oxide negative electrode material.
2. The method for preparing a pre-lithiated silicon monoxide negative electrode material according to claim 1, wherein in the step (1), the silicon monoxide powder is commercial silicon monoxide powder, and the particle size d50Is 0.1-10 μm.
3. The method for preparing the pre-lithiated silicon oxide negative electrode material according to claim 1, wherein in the step (2), the ratio of the silicon oxide powder to the lithium carbonate powder is 2: 1-8: 1.
4. The method for preparing the pre-lithiated silicon monoxide negative electrode material according to claim 1, wherein in the step (2), the mixing speed of the mixer is 200rpm, and the mixing time is 2 hours.
5. The method as claimed in claim 1, wherein the temperature of the heat treatment reaction in step (3) is 600-1100 ℃, and the reaction time is 3-7 hours.
6. The method as claimed in claim 1, wherein in step (3), the inert gas is one or more of nitrogen, argon and helium, and the aeration rate of the inert gas is 100-200 mL/min.
7. The method for preparing the pre-lithiated silicon oxide negative electrode material according to claim 1, wherein in the step (4), the carbon source gas is one or a mixture of acetylene, ethylene, methane and ethane.
8. The method as claimed in claim 1, wherein in the step (4), the carbon coating temperature is 650-850 ℃, and the coating time is 1-3 hours.
9. A prelithiated silicon oxide negative electrode material produced by the production method as claimed in any one of claims 1 to 8.
10. Use of the prelithiated silicon oxide anode material of claim 9 as an anode material for a lithium ion battery.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113023738A (en) * | 2021-03-03 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Silicon-based composite material, preparation method thereof and battery |
| CN114551872A (en) * | 2022-01-19 | 2022-05-27 | 惠州市豪鹏科技有限公司 | Negative electrode material, preparation method thereof, battery negative electrode and battery |
| CN114804118A (en) * | 2021-01-29 | 2022-07-29 | 中国科学技术大学 | Modified silicon monoxide material, preparation method thereof and lithium ion battery |
| CN115986094A (en) * | 2023-03-01 | 2023-04-18 | 江苏正力新能电池技术有限公司 | Pre-lithiated silicon oxide negative electrode material with core-shell structure and preparation method and application thereof |
| CN116632183A (en) * | 2023-03-16 | 2023-08-22 | 浙江锂宸新材料科技有限公司 | Method for continuously producing silicon-oxygen anode material with uniform carbon coating, product and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114804118A (en) * | 2021-01-29 | 2022-07-29 | 中国科学技术大学 | Modified silicon monoxide material, preparation method thereof and lithium ion battery |
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| CN115986094A (en) * | 2023-03-01 | 2023-04-18 | 江苏正力新能电池技术有限公司 | Pre-lithiated silicon oxide negative electrode material with core-shell structure and preparation method and application thereof |
| CN116632183A (en) * | 2023-03-16 | 2023-08-22 | 浙江锂宸新材料科技有限公司 | Method for continuously producing silicon-oxygen anode material with uniform carbon coating, product and application thereof |
| CN116632183B (en) * | 2023-03-16 | 2024-02-20 | 浙江锂宸新材料科技有限公司 | Method for continuously producing silicon-oxygen anode material with uniform carbon coating, product and application thereof |
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Application publication date: 20201204 |