CN112289997A - Silicon dioxide-based composite negative electrode material for lithium ion battery and preparation method thereof - Google Patents
Silicon dioxide-based composite negative electrode material for lithium ion battery and preparation method thereof Download PDFInfo
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Abstract
The invention provides a silicon dioxide-based composite negative electrode material for a lithium ion battery and a preparation method thereof, belonging to the field of negative electrode materials of lithium ion batteries. The problems of low first coulombic efficiency, low capacity output and the like caused by poor conductivity, large volume expansion and difficult conversion of silicon dioxide to silicon of the conventional silicon dioxide cathode material are solved. The invention adopts a simple mechanical ball milling method to mechanically mix the silicon dioxide, the transition metal simple substance powder and the carbon material at a high speed for a long time to form the composite material. SiO prepared by the invention2Fe/C composite material and metalThe half-cell prepared by matching Li has high initial coulombic efficiency, high discharge capacity, good cycle stability and rate capability, and the full-cell matched with the commercial NCM622 ternary cathode material also has good electrochemical performance.
Description
Technical Field
The invention belongs to the field of lithium ion battery cathode materials, and particularly relates to a silicon dioxide-based composite cathode material for a lithium ion battery and a preparation method thereof.
Background
Lithium ion batteries have been widely used in many fields such as portable electronic devices and electric vehicles, and have the advantages of high energy density, no memory effect, long cycle life, and the like. However, the theoretical specific capacity of the commercial graphite negative electrode widely used at present is only 372mAh g-1And the development of high-capacity and high-power lithium ion batteries is severely restricted, so that the development of high-specific-capacity cathode materials is imminent. At present, high-specific-capacity cathode materials such as silicon-based, tin-based, antimony-based and transition metal oxides are widely researched, but the high-specific-capacity cathode materials have the defects of high raw material price, serious volume expansion in the lithium desorption process of the materials, low first coulombic efficiency and the like, and the development of the high-specific-capacity cathode materials is severely limited. The silicon dioxide cathode material has rich raw material reserves, low price, easy preparation and as high as 1965mAh g-1The material has many advantages such as high theoretical specific capacity and the like, and is hopeful to become a next-generation high-cost performance anode material for replacing graphite. However, it also has problems of poor conductivity, large volume expansion, low first coulombic efficiency due to difficulty in conversion of silica to silicon (difficulty in breaking of siloxane bond), difficulty in sufficiently developing capacity, and the like. Currently, relatively few researches are carried out, and only patent CN110526251A discloses a method for preparing a size-controllable silica nanotube negative electrode material for a lithium ion battery by using a sol-gel method, wherein the material can relieve volume expansion and has high stability. But the method does not play a good role in improving the problems of low first coulombic efficiency, low capacity exertion and the like caused by poor inherent conductivity of the silicon dioxide cathode material and difficult conversion to silicon, and the used sol-gel synthesis method has complicated processes and is not beneficial to large-scale production.Therefore, the design of the silicon dioxide-based cathode material with high electronic conductivity, high silicon dioxide to silicon conversion efficiency and low volume expansion rate is very important, and meanwhile, the simple, feasible and low-cost preparation method is also beneficial to the large-scale production of the silicon dioxide cathode material, and the combination of the two advantages has important significance for the wide application of the silicon dioxide cathode material.
Disclosure of Invention
The invention aims to provide a silicon dioxide-based composite negative electrode material for a lithium ion battery and a preparation method thereof,
the cathode material has excellent charge-discharge cycle performance, rate performance and full battery performance.
The invention firstly provides a silicon dioxide-based composite negative electrode material for a lithium ion battery, which is obtained by ball-milling and mixing silicon dioxide, transition metal simple substance powder and a carbon material.
Preferably, the mass ratio of the silicon dioxide, the transition metal simple substance powder and the carbon material is (5-9): (0.5-3): (0.5-2).
Preferably, the mass ratio of the silicon dioxide, the transition metal simple substance powder and the carbon material is 7:2: 1.
preferably, the silica is silica spheres or silica tubes with the size of 10nm-10 μm.
Preferably, the elemental transition metal powder comprises Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Ta, W, Re, Ir, Pt, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or Lu.
Preferably, the size of the transition metal elementary powder material is 10nm-10 μm.
Preferably, the carbon material is acetylene black, artificial graphite, natural graphite, hard carbon or organic pyrolytic carbon.
Preferably, in the ball milling process, the ball-to-material ratio is (20:1) - (100: 1).
Preferably, in the ball milling process, the ball milling time is 10-25 h.
The invention also provides a preparation method of the silicon dioxide-based composite negative electrode material for the lithium ion battery, which comprises the following steps:
the method comprises the following steps: putting silicon dioxide, transition metal simple substance and carbon material into a planetary ball milling tank;
step two: and putting the ball milling beads into a planetary ball milling tank to be ground and mixed with the material to obtain the silicon dioxide/transition metal/carbon ternary composite negative electrode material.
The invention has the advantages of
The invention provides a silicon dioxide-based composite negative electrode material for a lithium ion battery and a preparation method thereof. The carbon matrix with soft texture is beneficial to relieving the volume expansion of the silicon dioxide; the composite material is compounded with the transition metal, so that the electronic conductivity of the silicon dioxide can be increased, the silicon-oxygen bond of the silicon dioxide and the lithium-oxygen bond of the lithium silicate can be catalyzed to break after the transition metal simple substance is tightly combined with the silicon dioxide, the activation energy required by bond breaking is reduced, more silicon dioxide can be converted into a silicon active material with high lithium storage capacity, and the first coulombic efficiency and the output specific capacity are improved. The experimental results show that: SiO prepared by the method2200mA g of Fe/C ternary composite material in the voltage range of 0.01-3.0V-1The first discharge specific capacity under the current density is 1119.6mAh g-1The first turn coulombic efficiency was 70.4%. At 200mA g-1The output specific capacity of the capacitor is 610mAh g after the capacitor is cycled for 200 times under the current density-1At 5A g-1The specific capacity of 308.6mAh g can be output under high current density-1. And the product is matched with a commercial NCM622 ternary positive material to be matched with a full battery, and the output specific capacity is 145.5mAh g after the product is cycled for 200 times under the current density of 0.5C-1The capacity retention rate can reach 78.5 percent, and the specific capacity can be output to 112mAh g under the 5C high current density-1. The silicon dioxide-based composite negative electrode material prepared by the method has good electrochemical lithium storage property, can be widely applied to negative electrode materials of lithium ion batteries, and is suitable for popularization and application.
Drawings
FIG. 1 shows SiO obtained in example 12XRD spectrogram of the/Fe/C ternary composite negative electrode material.
FIG. 2 shows SiO obtained in example 12SEM, TEM and EDS pictures of the/Fe/C ternary composite anode material. Wherein a is SiO as obtained in example 12SEM pictures of the/Fe/C ternary composite negative electrode material; b is SiO as obtained in example 12TEM pictures of the/Fe/C ternary composite negative electrode material; c is SiO as obtained in example 12HRTEM picture of the/Fe/C ternary composite negative electrode material; d is SiO as obtained in example 12EDS (electron-dispersive spectroscopy) spectrum pictures of the/Fe/C ternary composite anode material.
FIG. 3 shows SiO obtained in example 12the/Fe/C ternary composite negative electrode material is applied to a lithium half battery in a voltage range of 0.01-3.0V and at a voltage of 200mA g-1First charge and discharge curves at current density.
FIG. 4 shows that the voltage of the silicon dioxide-based ternary composite negative electrode material obtained in examples 1-3 and comparative examples 1-2 is in the range of 0.01-3.0V and 200mA g for a lithium half cell-1Graph of cycling stability at current density.
FIG. 5 shows SiO obtained in example 12A multiplying power performance test chart of the/Fe/C ternary composite negative electrode material in a voltage range of 0.01-3.0V.
FIG. 6 shows SiO obtained in example 12And a full battery electrochemical performance diagram of matching of the/Fe/C ternary composite cathode material and a commercial NCM622 ternary cathode material. Wherein a is a cyclic stability test chart at a current density of 0.5C; and b is a multiplying power performance test chart.
Detailed Description
Other aspects, features and advantages of the present invention will become apparent from the following detailed description, which, when taken in conjunction with the drawings, illustrate by way of example the principles of the invention. But this example does not limit the invention.
Example 1
1) Weighing 1.4g of 10-micron silicon dioxide balls, 0.4g of 5-10-micron iron powder and 0.2g of acetylene black according to the mass ratio of 7:2:1, and placing the silicon dioxide balls, the 0.4g of micron iron powder and the 0.2g of acetylene black in a low-energy planetary ball milling tank.
2) Weighing zirconia ball-milling beads according to the ball material mass ratio of 50:1, and mixing the zirconia ball-milling beads with the material obtained in the step 1).
3) The mixture is actually ball milled for 20 hours by utilizing a planetary ball mill and then taken out to obtain SiO2the/Fe/C ternary composite negative electrode material.
The resulting SiO2The XRD pattern of the/Fe/C ternary composite anode material is shown in figure 1, and a broad peak is formed at 22 degrees, and is a characteristic peak of typical amorphous silicon dioxide and carbon. The other two obvious peaks are characteristic peaks of the iron simple substance, which accord with 65-4855PDF cards, and no impurity peak exists.
The resulting SiO2The SEM test results of the/Fe/C ternary composite anode material are shown in fig. 2a, and it can be seen that it is a uniform mixture, indicating that silica, iron and carbon are uniformly compounded. FIG. 2b is the TEM result, and it can be seen that some fine particles are attached to the surface of the silica. Fig. 2c shows HRTEM, which shows that the simple substance Fe attached to the surface of silica has a distinct and good 110 crystal plane. FIG. 2d is the EDS spectrum, which shows the uniform distribution of four elements, Si, O, Fe and C.
Example 2
The preparation process and conditions were the same as in example 1, except that: replacing 0.4g of micron iron powder with the size of 5-10 mu m with 0.4g of micron nickel powder with the size of about 5 mu m in the step 1), and obtaining the SiO by the same operation2the/Ni/C ternary composite negative electrode material is used for investigating the catalytic capacities of different transition metal simple substances.
Example 3
The preparation process and conditions were the same as in example 1, except that: replacing 0.4g of micron iron powder with the size of 5-10 mu m with 0.4g of micron copper powder with the size of about 5 mu m in the step 1), and obtaining SiO by the same operation for the rest of the steps2the/Cu/C ternary composite cathode material is used for inspecting the catalytic capability of different transition metal simple substances.
Comparative example 1
The preparation method and conditions were the same as in step 2) and step 3) of example 1, except that: in the step 1), no transition metal simple substance is added1.4g of silica balls with the size of 10 mu m and 0.6g of acetylene black are weighed according to the mass ratio of 7:3 and put into a low-energy planetary ball milling tank to obtain SiO2the/C binary composite negative electrode material is compared with the above-mentioned examples with transition metals.
Comparative example 2
The preparation process was carried out under the same conditions as in step 2) and step 3) of example 1, except that: in the step 1), no transition metal simple substance and carbon are added, only 2.0g of silicon dioxide balls with the size of 10 mu m are weighed and placed in a low-energy planetary ball milling tank, and ball-milled SiO is obtained2Negative electrode material, in comparison with the above examples with transition metal and carbon.
Application example 1
The silica-based composite anode materials prepared in examples 1 to 3 and comparative examples 1 to 2 were subjected to electrochemical lithium storage performance tests. The method comprises the following specific steps:
weighing the negative electrode active material, acetylene black and CMC according to the mass ratio of 7:2:1, putting the materials into an agate mortar, mixing the materials in a water solvent, grinding the materials for 30 minutes, coating the materials on a copper foil, drying the copper foil in an oven at 80 ℃, and completely drying the copper foil in a vacuum oven after rolling and cutting. The counter electrode adopts a metal lithium sheet, the diaphragm is a polypropylene porous membrane, and the electrolyte adopts 1mol L-1LiPF of6Lithium salt is dissolved in an EC/DMC/FEC solvent system with the volume ratio of 45/45/10, a 2025 type button cell is adopted as a battery, and lithium storage performance test is carried out in a voltage range of 0.01-3V.
SiO obtained in example 12The battery prepared from the/Fe/C ternary composite cathode material is 200mAg-1The first charge-discharge curve under the current density is shown in figure 3, the first coulombic efficiency can reach 70.4%, and the first charge-discharge specific capacity is 788.6mAh g respectively-1And 1119.6mAh g-1. The charge-discharge cycle performance test of the batteries prepared from the materials obtained in examples 1-3 and comparative examples 1-2 is shown in fig. 4, and comparative analysis shows that: at 200mAg-1At current density, the material of example 1 had the highest discharge capacity of 610mAh g after 200 cycles-1. FIG. 5 shows the rate capability of the example 1 material at 5A g-1The specific capacity which can be output under high current density is 308.6mAh g-1. The silicon dioxide/transition metal simple substance/carbon ternary composite material obtained by the method has excellent electrochemical performance, so that the method has more commercial popularization superiority.
Application example 2
The material obtained in example 1 is matched with a commercial NCM622 positive electrode material to carry out an electrochemical lithium storage performance test on a full cell, and the specific steps are as follows:
the electrode sheet of the material of example 1 prepared in application example 1 above was used and pre-lithiated beforehand to improve the coulombic efficiency. The preparation process of the commercial NCM622 positive electrode material electrode plate is as follows: mixing the positive active material, Super P and PVDF in a solvent of N-methyl pyrrolidone (NMP) according to a mass ratio of 90:5:5, uniformly mixing by using a homogenizer, coating on an aluminum foil, drying in a drying oven at 120 ℃, rolling and cutting into pieces, and completely drying in a vacuum drying oven. The diaphragm is a polypropylene porous membrane, and 1mol L of electrolyte is adopted-1LiPF of6Lithium salt is dissolved in an EC/DMC/FEC solvent system with the volume ratio of 45/45/10, the battery adopts a 2025 type button cell, SiO2And the/Fe/C cathode is used for carrying out lithium storage performance test on the commercial NCM622 positive electrode full cell in a voltage range of 0.5-4.3V.
The charge-discharge cycle performance and rate performance test of the material obtained in example 1 matched with the commercial NCM622 positive electrode material for a full cell is shown in FIG. 6, and the specific capacity of the material is 145.5mAh g after 200 cycles under the current density of 0.5C-1The capacity retention rate can reach 78.5 percent, and the specific capacity of 112mAh g can be output under the high current density of 5C-1. This fully illustrates the SiO obtained in example 12the/Fe/C ternary composite negative electrode material also shows good electrochemical performance in a full cell, and is not limited to a lithium half cell, so that the invention has practical significance in wide application.
The present invention includes, but is not limited to, the above embodiments, and any equivalent substitutions or partial modifications made under the principle of the spirit of the present invention are considered to be within the scope of the present invention.
Claims (10)
1. The silicon dioxide-based composite negative electrode material for the lithium ion battery is characterized by being obtained by ball-milling and mixing silicon dioxide, transition metal simple substance powder and a carbon material.
2. The silicon dioxide-based composite anode material for the lithium ion battery according to claim 1, wherein the mass ratio of the silicon dioxide to the transition metal elemental powder to the carbon material is (5-9): (0.5-3): (0.5-2).
3. The silicon dioxide-based composite anode material for the lithium ion battery according to claim 2, wherein the mass ratio of the silicon dioxide to the transition metal elemental powder to the carbon material is 7:2: 1.
4. the silicon dioxide-based composite anode material for the lithium ion battery according to claim 1, wherein the silicon dioxide is a silicon dioxide sphere or a silicon dioxide tube, and the size of the silicon dioxide is 10nm-10 μm.
5. The silica-based composite anode material for lithium ion batteries according to claim 1, wherein the elemental transition metal powder comprises Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Ta, W, Re, Ir, Pt, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or Lu.
6. The silicon dioxide-based composite anode material for the lithium ion battery according to claim 1 or 5, wherein the size of the transition metal elemental powder material is 10nm-10 μm.
7. The silicon dioxide-based composite negative electrode material for the lithium ion battery according to claim 1, wherein the carbon material is acetylene black, artificial graphite, natural graphite, hard carbon or organic pyrolytic carbon.
8. The silicon dioxide-based composite anode material for the lithium ion battery according to claim 1, wherein the ball-to-material ratio in the ball milling process is (20:1) - (100: 1).
9. The silicon dioxide-based composite anode material for the lithium ion battery according to claim 1, wherein the ball milling time is 10-25 hours in the ball milling process.
10. The preparation method of the silica-based composite anode material for the lithium ion battery according to claim 1, characterized by comprising the following steps:
the method comprises the following steps: putting silicon dioxide, transition metal simple substance and carbon material into a planetary ball milling tank;
step two: and putting the ball milling beads into a planetary ball milling tank to perform ball milling and mixing with the material to obtain the silicon dioxide/transition metal/carbon ternary composite negative electrode material.
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| WO2023065128A1 (en) * | 2021-10-19 | 2023-04-27 | 宁德时代新能源科技股份有限公司 | Negative electrode sheet, secondary battery, battery module, battery pack, and electric device |
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