CN112289985B - C @ MgAl2O4Composite coating modified silicon-based negative electrode material and preparation method thereof - Google Patents
C @ MgAl2O4Composite coating modified silicon-based negative electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses C @ MgAl2O4A composite coated modified silicon-based negative electrode material and a preparation method thereof relate to the technical field of electrochemical energy storage, and the material comprises a silicon-based negative electrode material and MgAl sequentially coated on the surface of the silicon-based negative electrode material2O4A coating layer and a carbon coating layer; the preparation process comprises the following steps: preparing Al (NO)3)3·9H2O and Mg (NO)3)2·6H2Mixing the O aqueous solution, adding a crosslinking monomer, a crosslinking agent and an initiator, and heating to react to prepare gel; performing ball milling treatment on the silicon-based negative electrode material to obtain slurry, adding gel into the slurry, stirring and dispersing in vacuum, and performing spray drying to obtain a precursor of the silicon-based negative electrode material; calcining the silicon-based anode material precursor at high temperature in the air atmosphere to obtain MgAl2O4Coating the modified silicon-based negative electrode material, and calcining the coated silicon-based negative electrode material in a mixed atmosphere containing acetylene to obtain the silicon-based negative electrode material. C @ MgAl prepared by the invention2O4The composite coated and modified silicon-based negative electrode material has a stable structure and small volume expansion in the charging and discharging processes, and improves the first coulombic efficiency and the cycling stability of the material.
Description
Technical Field
The invention relates to the technical field of electrochemical energy storage, in particular to a C@MgAl2O4A composite coating modified silicon-based negative electrode material and a preparation method thereof.
Background
With the rapid development of electric vehicles, energy storage power stations, portable electronic devices, and the like, lithium ion batteries with high specific energy are receiving more and more attention. Because the reversible specific capacity of the anode material has a small lifting space, the lifting of the reversible specific capacity of the cathode material is the key for improving the energy density of the lithium ion battery at present. However, the current commercial lithium ion battery cathode material is mainly graphite carbon cathode material, and the theoretical specific capacity is only 372mAh/g (LiC)6) Further development of lithium ion batteries is severely limited. The silicon-based material is a research system with higher theoretical specific capacity in the negative electrode material, and the formed alloy is LixSi (x ═ 0-4.4), with a theoretical specific capacity of up to 4200mAh/g, is considered an ideal substitute product for carbon negative electrode materials due to its low intercalation potential, low atomic mass, high energy density and high Li mole fraction in Li-Si alloys. However, the silicon negative electrode shows poor cycle performance due to the destruction and mechanical pulverization of the material structure due to its severe volume expansion and contraction during the intercalation and deintercalation of lithium. SiO has poor conductivity and properties close to an insulator, so that the electrochemical reaction has poor kinetic performance, and SiO contained in the SiO material2Conversion to Li in a first lithium insertion reaction4SiO4、Li2Si2O5And the phases are equivalent, so that more lithium ions are consumed, and the first charge-discharge efficiency is lower. The mainstream commercial silicon oxide composite negative electrode material is generally coated with carbon, so that the conductivity of the material is improved, meanwhile, the silicon oxide material is prevented from being directly contacted with electrolyte, and the cycle performance of the material is improved. However, the large-scale application of the silicon-based negative electrode material still faces a lot of tests, the cycle performance of the material is further improved, the first coulombic efficiency of the material is improved, the production cost is reduced, and the majority of researchers and manufacturers still pay great care and distance.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for improving the stability of a cableC@MgAl2O4The composite coated and modified silicon-based negative electrode material and the preparation method thereof have the advantages that the negative electrode material is stable in structure and small in volume expansion in the charging and discharging processes, and the first coulomb efficiency and the circulation stability of the silicon-based negative electrode material are improved.
The invention provides C @ MgAl2O4The composite coated modified silicon-based negative electrode material comprises a silicon-based negative electrode material and MgAl sequentially coated on the surface of the silicon-based negative electrode material2O4A coating layer and a carbon coating layer.
Preferably, the C @ MgAl2O4In the composite modified silicon-based negative electrode material, MgAl2O4The mass percentage of the coating layer is 0.5-5%, and the mass percentage of the carbon coating layer is 0.5-5%.
Preferably, the silicon-based anode material is a commercially pure silica anode material or a nano-silicon anode material.
The invention also provides the C @ MgAl2O4The preparation method of the composite coating modified silicon-based negative electrode material comprises the following steps:
s1, preparation of Al (NO)3)3·9H2O and Mg (NO)3)2·6H2Mixing the water solution of O, adding a crosslinking monomer, a crosslinking agent and an initiator, and heating to react to prepare gel;
s2, performing ball milling treatment on the silicon-based negative electrode material to obtain slurry, adding gel into the slurry, stirring and dispersing in vacuum, and performing spray drying to obtain a precursor of the silicon-based negative electrode material;
s3, calcining the silicon-based anode material precursor at high temperature in the air atmosphere to obtain MgAl2O4Coating the modified silicon-based negative electrode material;
s4, using acetylene as carbon source and MgAl2O4Calcining the coated and modified silicon-based negative electrode material in a mixed atmosphere containing acetylene to obtain C @ MgAl2O4And compounding and coating the modified silicon-based negative electrode material.
Preferably, in S1, the crosslinking monomer is acrylamide, the crosslinking agent is N, N' -methylenebisacrylamide, and the initiator is ammonium persulfate; preferably, the temperature is raised to 60-100 ℃ and the reaction is carried out for 3-6 h.
Preferably, in S2, the spray drying temperature is 120-200 ℃.
Preferably, in S3, the calcination temperature is 700-900 ℃, the temperature rise speed is 3-10 ℃/min, and the calcination time is 2-5 h.
Preferably, in S4, the mixed atmosphere is a nitrogen-acetylene mixed atmosphere, wherein the volume percentage of acetylene is 40-50%.
Preferably, in S4, the calcination temperature is 750-950 ℃, the temperature rise rate is 3-10 ℃/min, and the calcination time is 1-3 h.
Compared with the prior art, the beneficial effects of the invention are embodied in the following aspects:
1. firstly, a layer of MgAl is coated on a silicon-based negative electrode material2O4The coating material is prepared by a polymer network gel method through calcination, has good chemical stability, has a porous structure and good matching performance with silicon, and can effectively relieve the problem of volume expansion of Si and SiO in the process of lithium intercalation and deintercalation; and then carbon coating is carried out to effectively improve the conductivity of the alloy.
2. C @ MgAl prepared by the invention2O4The composite coated and modified silicon-based negative electrode material has a stable structure and small volume expansion in the charging and discharging processes, and improves the first coulombic efficiency and the cycling stability of the material.
3. The preparation method is simple and feasible, low in cost, environment-friendly and easy to realize industrial production.
Drawings
Fig. 1 is a first charging and discharging curve diagram of charging prepared from a silicon-based negative electrode material in example 1 of the present invention; wherein curve a is SiOx@MgAl2O4@ C silicon-based negative electrode material, curve b is uncoated modified SiOxAnd (3) a silicon-based negative electrode material.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
C @ MgAl2O4Preparing a composite modified silicon-based negative electrode material:
(1) with Al (NO)3)3·9H2O and Mg (NO)3)2·6H2Preparing water solution with O as raw material, wherein Al (NO)3)3·9H2O and Mg (NO)3)2·6H2The molar ratio of O is 2: 1 (wherein Al (NO)3)3·9H2O and Mg (NO)3)2·6H2The mass of O is 10.7586g and 3.6768g respectively), 4g of acrylamide monomer, 4g of crosslinking agent N, N' -methylene-bisacrylamide and 1g of initiator ammonium persulfate are added into the aqueous solution respectively, and the gel is obtained after 5 hours of polymerization at 80 ℃.
(2) 100g of commercial SiO are takenxPlacing the powder in a ball milling tank for ball milling to obtain slurry, adding gel for vacuum stirring and dispersing, and performing spray drying to obtain a silicon-based anode material precursor, wherein the drying temperature is 180 ℃;
(3) placing the mixture after spray drying in a tubular furnace for high-temperature calcination in the atmosphere of air at 800 ℃, at a temperature-rise speed of 5 ℃/min for 3h to obtain 2% MgAl2O4A modified silicon-based negative electrode material; and then continuing to perform C coating in a tubular furnace, wherein the tubular furnace is a nitrogen-acetylene mixed atmosphere, the coating temperature is 800 ℃, the heating rate is 5 ℃/min, the flow rate of the mixed gas is 200L/h, and the coating time is 2h, the volume of acetylene in the mixed atmosphere accounts for 50%, and after coating, naturally cooling to room temperature to obtain C @ MgAl2O4Composite coating modified silicon-based negative electrode material (SiO)x@MgAl2O4@C)。
For the SiO obtained in example 1x@MgAl2O4The electrochemical performance of the @ C silicon-based negative electrode material is tested, and FIG. 1 shows SiO of example 1x@MgAl2O4@ C silicon-based negative electrode material and commercial SiO without coating treatmentxFirst charge and discharge curves under the conditions of 0.05C multiplying factor (1C is 1300mA/g) and voltage interval of 0.05-1.5V. Among them, commercial SiOxThe first discharge specific capacity is 1649.43mAh/g, and the charge specific capacity is703.58 mAh/g, the first coulombic efficiency is only 42.66%. And SiOx@MgAl2O4The @ C material has the first discharge specific capacity of 2020.42mAh/g, the charge specific capacity of 1495.62mAh/g and the first coulombic efficiency of 74.03 percent, shows higher first effect and first charge specific capacity, and has great significance for improving the capacity and the first effect of the full battery. At the same time, SiOx@MgAl2O4The discharge platform of the @ C material is significantly lower than that of commercial SiOxShows less polarization. Thus, compared to untreated commercial SiOxMaterial, SiOx@MgAl2O4The @ C material has the advantages of high specific capacity, first effect, small polarization and good electrochemical performance.
Example 2
C @ MgAl2O4Preparing a composite modified silicon-based negative electrode material:
(1) with Al (NO)3)3·9H2O and Mg (NO)3)2·6H2Preparing water solution with O as raw material, wherein Al (NO)3)3·9H2O and Mg (NO)3)2·6H2The molar ratio of O is 2: 1 (wherein Al (NO)3)3·9H2O and Mg (NO)3)2·6H2The mass of O is 10.7586g and 3.6768g respectively), 4g of acrylamide monomer, 4g of crosslinking agent N, N' -methylene-bisacrylamide and 1g of initiator ammonium persulfate are added into the aqueous solution respectively, and the gel is obtained after polymerization is carried out for 6 hours at the temperature of 60 ℃.
(2) 40g of commercial SiO are takenxPutting the powder into a ball milling tank, performing ball milling to obtain slurry, adding gel, performing vacuum stirring and dispersion, and performing spray drying to obtain a silicon-based anode material precursor, wherein the drying temperature is 130 ℃;
(3) placing the mixture after spray drying in a tubular furnace for high-temperature calcination in the atmosphere of air at 700 ℃, at a heating rate of 3 ℃/min for 5h to obtain 5% MgAl2O4A modified silicon-based negative electrode material; then, C coating is continuously carried out in a tubular furnace, the tubular furnace is in a nitrogen acetylene mixed atmosphere, the coating temperature is 850 ℃,the heating rate is 5 ℃/min, the flow rate of the mixed gas is 200L/h, the coating time is 2.5h, the volume percentage of acetylene in the mixed atmosphere is 40%, and the mixture is naturally cooled to the room temperature after coating to obtain C @ MgAl2O4Composite coating modified silicon-based negative electrode material (SiO)x@MgAl2O4@C)。
Example 3
C @ MgAl2O4Preparing a composite modified silicon-based negative electrode material:
(1) with Al (NO)3)3·9H2O and Mg (NO)3)2·6H2Preparing water solution with O as raw material, wherein Al (NO)3)3·9H2O and Mg (NO)3)2·6H2The molar ratio of O is 2: 1 (wherein Al (NO)3)3·9H2O and Mg (NO)3)2·6H2The mass of O is 10.7586g and 3.6768g respectively), 4g of acrylamide monomer, 4g of crosslinking agent N, N' -methylene-bisacrylamide and 1g of initiator ammonium persulfate are added into the aqueous solution respectively, and the gel is obtained after 3 hours of polymerization at the temperature of 100 ℃.
(2) 400g of commercial SiO are takenxPutting the powder into a ball milling tank, performing ball milling to obtain slurry, adding gel, performing vacuum stirring and dispersion, and performing spray drying to obtain a silicon-based anode material precursor, wherein the drying temperature is 200 ℃;
(3) placing the mixture after spray drying in a tubular furnace for high-temperature calcination in the atmosphere of air at 900 ℃, at a heating rate of 10 ℃/min for 2h to obtain 0.5 percent MgAl2O4A modified silicon-based negative electrode material; and then continuing to perform C coating in a tubular furnace, wherein the tubular furnace is a nitrogen-acetylene mixed atmosphere, the coating temperature is 950 ℃, the heating rate is 10 ℃/min, the flow rate of the mixed gas is 200L/h, the coating time is 1h, the volume ratio of acetylene in the mixed atmosphere is 45%, and the mixture is naturally cooled to room temperature after coating to obtain C @ MgAl2O4Composite coating modified silicon-based negative electrode material (SiO)x@MgAl2O4@C)。
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. C @ MgAl2O4The preparation method of the composite coated and modified silicon-based negative electrode material is characterized by comprising the silicon-based negative electrode material and MgAl coated on the surface of the silicon-based negative electrode material in sequence2O4A coating layer and a carbon coating layer;
the method specifically comprises the following steps:
s1, preparation of Al (NO)3)3·9H2O and Mg (NO)3)2·6H2Mixing the water solution of O, adding a crosslinking monomer, a crosslinking agent and an initiator, and heating to react to prepare gel; the crosslinking monomer is acrylamide, the crosslinking agent is N, N' -methylene bisacrylamide, and the initiator is ammonium persulfate; the temperature rise reaction temperature is 60-100 ℃, and the reaction time is 3-6 h;
s2, performing ball milling treatment on the silicon-based negative electrode material to obtain slurry, adding gel into the slurry, stirring and dispersing in vacuum, and performing spray drying to obtain a precursor of the silicon-based negative electrode material; the spray drying temperature is 120-200 ℃;
s3, calcining the silicon-based anode material precursor at high temperature in the air atmosphere to obtain MgAl2O4Coating the modified silicon-based negative electrode material; the calcination temperature is 700-900 ℃, the heating rate is 3-10 ℃/min, and the calcination time is 2-5 h;
s4, using acetylene as carbon source and MgAl2O4Calcining the coated and modified silicon-based negative electrode material in a mixed atmosphere containing acetylene to obtain C @ MgAl2O4And compounding and coating the modified silicon-based negative electrode material.
2. C @ MgAl of claim 12O4The preparation method of the composite coating modified silicon-based anode material is characterized in that C @ MgAl2O4In the composite modified silicon-based negative electrode material, MgAl2O4The mass percentage of the coating layer is 0.5-5%, and the mass percentage of the carbon coating layer is 0.5-5%.
3. C @ MgAl of claim 12O4The preparation method of the composite coating modified silicon-based negative electrode material is characterized in that the silicon-based negative electrode material is a commercial pure silicon oxide negative electrode material or a nano silicon negative electrode material.
4. C @ MgAl of claim 12O4The preparation method of the composite coating modified silicon-based negative electrode material is characterized in that in S4, the mixed atmosphere is a nitrogen-acetylene mixed atmosphere, wherein the volume percentage of acetylene is 40-50%.
5. C @ MgAl of claim 12O4The preparation method of the composite coating modified silicon-based negative electrode material is characterized in that in S4, the calcining temperature is 750-950 ℃, the heating rate is 3-10 ℃/min, and the calcining time is 1-3 h.
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