CN115028169B - Preparation method of porous silicon monoxide negative electrode material for lithium ion battery - Google Patents
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a porous silicon monoxide negative electrode material for a lithium ion battery. Mixing silicon monoxide and sodium hydroxide, and pressing into a sheet to obtain a sheet composite material; carrying out heat treatment on the flaky composite material to obtain a product; and crushing the product, stirring in deionized water, washing with alcohol, and drying to obtain the porous silicon monoxide negative electrode material for the lithium ion battery. According to the invention, after the sodium hydroxide and the silicon monoxide are pressed into the tablet, the contact area of the sodium hydroxide and the silicon monoxide is increased, so that the reaction between the sodium hydroxide and the silicon monoxide is facilitated; and the obtained porous structure can effectively relieve larger volume expansion/shrinkage in the charging and discharging processes, and has excellent industrialized prospect.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a porous silicon monoxide negative electrode material for a lithium ion battery.
Background
Lithium Ion Batteries (LIBs) are widely used in our daily lives because of their high energy density, long cycle life, green and pollution-free characteristics. However, with the development of new energy automobiles and other fields, the traditional graphite (372 mAhg) -1 ) The lithium ion battery cathode material cannot meet the requirements of people on high-energy density batteries. Silicon and silicon oxide (SiO) x ,0<x<2) The method has the advantages of high theoretical specific capacity, rich reserves and the like, thereby attracting the attention of researchers. However, the silicon material will generate larger volume expansion/contraction during lithium intercalation/deintercalation, so that the active material is broken and pulverized, and the active material and the current collector are separated and fall off, thereby causing the rapid decline of the capacity. In addition, the large volume expansion also makes the electrode unable to generate a stable Solid Electrolyte Interface (SEI) film, irreversibly consumes lithium ions, resulting in the first coulombic efficiency of the electrode(ICE) is very low.
Chinese patent CN 102447112A discloses a silicon-carbon composite material, a preparation method thereof, and a negative electrode material and a lithium ion battery containing the silicon-carbon composite material, wherein the silicon-carbon composite material comprises hollow porous carbon spheres coating nano silicon particles, the particle size of the nano silicon particles in the silicon-carbon composite material is 5-80nm, and the content of nano silicon is 10-90wt%. The preparation method of the silicon-carbon composite material comprises the following steps: (1) preparing a polymer solution: dissolving high molecular polymer in solvent to obtain 1-20wt% polymer solution; and (2) uniformly mixing the silicon monoxide and the polymer: mixing silicon monoxide with the polymer solution obtained in the step (1) according to a proportion, fully dispersing, and removing the solvent to obtain a polymer-coated silicon monoxide composite material; (3) carrying out carbonization and disproportionation reaction at high temperature: heating the composite material of polymer coated with silicon monoxide obtained in the step (2) in a protective atmosphere to enable a high molecular polymer to generate a carbonization reaction and silicon monoxide to generate a disproportionation reaction, so as to obtain a porous carbon sphere coated silicon dioxide/nano silicon composite material; and (4) etching to remove silicon dioxide: and (4) mixing the porous carbon sphere coated silicon dioxide/nano silicon composite material obtained in the step (3) with corrosive liquid according to the mass ratio of 1: 5-1: 100, stirring for 0.5-24 hours, and separating to obtain the silicon-carbon composite material. In the patent, the silicon dioxide after disproportionation reaction is used as a template agent to prepare the porous carbon spheres, the disproportionation degree is not easy to control, so that the amount of the generated silicon dioxide cannot be accurately controlled, factors such as reaction time and the like need to be accurately mastered while the silicon dioxide is removed by corrosion, and otherwise, the silicon is easy to corrode.
Chinese patent CN 103413922A discloses a lithium ion battery negative electrode material and a preparation method thereof, wherein the negative electrode material comprises 20-100nm of primary particles and 50-170m of specific surface area 2 Silicon negative electrode material SiO composed of/g x Wherein x is more than 0 and less than 0.1. The preparation method comprises the steps of reacting silicon monoxide in an inert atmosphere at a constant temperature of 800-1100 ℃, cooling to room temperature after the reaction is finished, removing impurities through acid or alkali treatment, washing and drying to obtain silicon particles, and cooling to room temperature after the silicon particles are coated with carbon in the inert atmosphere. In the patent, the reaction at high temperature of 800 to 1100 ℃ consumes more energy, and the production is increasedThis is true.
SiO produces Li during intercalation 2 The O, lithium silicate can be used as a buffer medium to relieve the volume expansion of a part, but the expansion is still as high as 200 percent, and the rapid capacity decline is still caused, so that the commercialization process is influenced.
Disclosure of Invention
The invention aims to provide a preparation method of a porous silicon monoxide negative electrode material for a lithium ion battery, which has a simple synthesis process, and the prepared porous silicon monoxide negative electrode material for the lithium ion battery has good cycle stability and smaller volume expansion.
The preparation method of the porous silicon monoxide negative electrode material for the lithium ion battery is that silicon monoxide and sodium hydroxide are mixed and then pressed into a sheet shape to obtain a sheet-shaped composite material; carrying out heat treatment on the flaky composite material to obtain a product; and crushing the product, stirring in deionized water, washing with alcohol, and drying to obtain the porous silicon monoxide negative electrode material for the lithium ion battery.
The mass ratio of the silicon monoxide to the sodium hydroxide is 1.5-3:1.
The grain diameter of the silicon monoxide is 1-3 μm.
The mesh number of the sodium hydroxide is 300-600 meshes.
The mixing time is 40-60min.
The sheet shape is a circular sheet shape.
The diameter of the sheet-shaped composite material is 20-30mm.
The heat treatment temperature is 350-400 ℃, and the heat treatment time is 2-2.5h.
The stirring time is 12-20h.
The washing times are 3-5 times, and the washing times are 3-5 times.
The drying is vacuum drying, and the drying temperature is 80-100 ℃.
The preparation method of the porous silicon monoxide negative electrode material for the lithium ion battery comprises the following steps:
(1) Grinding sodium hydroxide in inert atmosphere, and sieving;
(2) Grinding and mixing the sodium hydroxide obtained in the step (1) and silicon monoxide in an inert atmosphere to obtain silicon monoxide/sodium hydroxide mixed powder;
(3) Pressing the silicon monoxide/sodium hydroxide mixed powder obtained in the step (2) into a sheet shape to obtain a sheet-shaped composite material;
(4) And (4) carrying out heat treatment on the sheet composite material obtained in the step (3) in an inert atmosphere to obtain a product, crushing the product, stirring the crushed product in deionized water, and washing with water, alcohol and drying to obtain the porous silicon monoxide negative electrode material for the lithium ion battery.
The inert atmosphere in the step (1) is nitrogen atmosphere or argon atmosphere.
And (3) the inert atmosphere in the step (2) is nitrogen atmosphere or argon atmosphere.
And (4) the inert atmosphere in the step (4) is nitrogen atmosphere or argon atmosphere.
The SiO is industrial grade SiO, and the purity of the SiO is more than 99wt%.
In order to solve the problems that the existing silicon monoxide used as a lithium ion battery cathode can generate larger volume expansion/contraction, cracking and pulverization when lithium is inserted and extracted, the invention heats sodium hydroxide and silicon monoxide with smaller particle size in inert atmosphere after mixing the sodium hydroxide and the silicon monoxide, and the silicon monoxide is etched into a porous structure by the reaction of the sodium hydroxide and the silicon monoxide in a molten state. The prepared porous silicon monoxide cathode material is used as a lithium ion battery cathode material, and the rich pore structure on the surface of the silicon monoxide can relieve larger stress generated during lithium intercalation and deintercalation, so that the silicon monoxide lithium ion battery cathode material with lower volume expansion, good cycle performance and other excellent electrochemical properties is obtained.
The invention provides a preparation method of a porous silicon monoxide negative electrode material for a lithium ion battery for relieving volume expansion. According to the invention, the pore structure is prepared on the surface of the silicon monoxide by sodium hydroxide etching, so that the volume expansion/contraction of the silicon monoxide during lithium intercalation/deintercalation can be relieved, and the cathode material is prevented from being pulverized and broken due to volume expansion, thereby improving the electrochemical performance of the silicon monoxide as the cathode material.
The porous silicon monoxide negative electrode material prepared by the invention is used as a negative electrode active material of a lithium ion battery.
The porous silicon monoxide negative electrode material prepared by the invention is applied as follows:
(1) The porous silicon monoxide negative electrode material, the conductive agent and the binder are stirred and mixed to prepare slurry; the conductive agent and the adhesive are both made of materials known in the industry;
(2) Coating the slurry on the surface of the current collector to obtain a negative electrode; the current collector is a material well known in the industry;
(3) And (3) assembling the cathode, the anode, the diaphragm and the electrolyte obtained in the step (2) into the lithium ion battery.
The porous silicon monoxide negative electrode material is prepared by utilizing the principle that the melting points of silicon monoxide and sodium hydroxide are different and the melting point of the sodium hydroxide is lower than that of the silicon monoxide. The silicon monoxide and sodium hydroxide are ground and mixed in an inert atmosphere, and after the mixture is pressed into a sheet layer, the sodium hydroxide at high temperature is changed into a molten state through heat treatment in the inert atmosphere and fully reacts with the silicon monoxide in close contact, so that the surface of the silicon monoxide is etched to form the porous silicon monoxide material.
The porous silicon monoxide lithium ion battery cathode material is prepared by a molten sodium hydroxide etching method, and the lithium ion battery cathode material with good cycling stability and small volume expansion can be obtained by the method.
The invention has the following beneficial effects:
aiming at the problem that the volume expansion of the existing silicon monoxide cathode is large, after sodium hydroxide and silicon monoxide are pressed into tablets, the contact area of the sodium hydroxide and the silicon monoxide is increased, so that the reaction between the sodium hydroxide and the silicon monoxide is facilitated; then heating reaction is carried out, and one-step forming can be realized. The invention has simple synthesis process and low heat treatment temperature, and the obtained porous structure can effectively relieve larger volume expansion/contraction in the charge-discharge process, thereby having excellent industrialization prospect.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Fig. 2 is a microscopic morphology image of the porous silicon monoxide negative electrode material for the lithium ion battery prepared in example 1, wherein the left image is a scanning electron microscope image, and the right image is a transmission electron microscope image.
Fig. 3 is a microscopic morphology image of the porous silicon monoxide negative electrode material for the lithium ion battery prepared in example 2, wherein the left image is a scanning electron microscope image, and the right image is a transmission electron microscope image.
Fig. 4 is a microscopic morphology image of the porous silicon monoxide negative electrode material for the lithium ion battery prepared in example 3, wherein the left image is a scanning electron microscope image, and the right image is a transmission electron microscope image.
FIG. 5 shows the cell performance at 0.01 to 2.5V and 100mAg for the cells of example 1, example 2, example 3 and comparative example 1 -1 Graph of cycling performance at current density.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
(1) Grinding sodium hydroxide in an argon (Ar) filled glove box, and then sieving through a 300-mesh sieve;
(2) Grinding and mixing 5g of silicon monoxide with the particle size of 1-3 mu m and the sodium hydroxide obtained after sieving in the step (1) in a glove box filled with argon (Ar) for 40min to obtain silicon monoxide/sodium hydroxide mixed powder; wherein the mass ratio of the silicon monoxide to the sodium hydroxide is 1.5;
(3) Pressing the silicon monoxide/sodium hydroxide mixed powder into a round sheet with the diameter of 20mm to obtain a sheet composite material;
(4) Placing the sheet composite material in a nickel crucible, and heating for 2 hours at 350 ℃ in an argon atmosphere to obtain a product; and crushing the product, stirring in a conical flask containing deionized water for 12h, respectively centrifugally washing with water and ethanol for 3 times, and finally drying in vacuum at 80 ℃ to obtain the porous silicon monoxide negative electrode material for the lithium ion battery, wherein the microscopic morphology of the porous silicon monoxide negative electrode material is shown in figure 2.
Example 2
(1) Grinding sodium hydroxide in a glove box filled with argon (Ar), and sieving with a 500-mesh sieve;
(2) Grinding and mixing 5g of silicon monoxide with the particle size of 1-3 mu m and the sodium hydroxide obtained after sieving in the step (1) in a glove box filled with argon (Ar) for 50min to obtain silicon monoxide/sodium hydroxide mixed powder; wherein the mass ratio of the silicon monoxide to the sodium hydroxide is 2:1;
(3) Pressing the silicon monoxide/sodium hydroxide mixed powder into a wafer with the diameter of 25mm to obtain a sheet composite material;
(4) Putting the sheet composite material into a nickel crucible, and heating for 2.5 hours at 370 ℃ under the argon atmosphere to obtain a product; and crushing the product, stirring in a conical flask containing deionized water for 20 hours, respectively centrifugally washing with water and ethanol for 4 times, and finally drying in vacuum at 90 ℃ to obtain the porous silicon monoxide negative electrode material for the lithium ion battery, wherein the microstructure of the porous silicon monoxide negative electrode material is shown in figure 3.
Example 3
(1) Grinding sodium hydroxide in an argon (Ar) filled glove box, and then sieving by using a 600-mesh sieve;
(2) Grinding and mixing 5g of silicon monoxide with the particle size of 1-3 mu m and the sodium hydroxide obtained after sieving in the step (1) in a glove box filled with argon (Ar) for 60min to obtain silicon monoxide/sodium hydroxide mixed powder; wherein the mass ratio of the silicon monoxide to the sodium hydroxide is 3:1;
(3) Pressing the silicon monoxide/sodium hydroxide mixed powder into a sheet with the diameter of 30mm to obtain a sheet composite material;
(4) Placing the sheet composite material in a nickel crucible, and heating for 2.2h at 400 ℃ under the argon atmosphere to obtain a product; and crushing the product, stirring for 18h in a conical flask containing deionized water, respectively centrifugally washing for 5 times by using water and ethanol, and finally drying in vacuum at 100 ℃ to obtain the porous silicon monoxide negative electrode material for the lithium ion battery, wherein the microscopic morphology of the porous silicon monoxide negative electrode material is shown in figure 4.
As can be seen from the SEM images and TEM images in fig. 2, 3 and 4, as the mass ratio of silicon monoxide to sodium hydroxide is varied from 1.5:1 to 3:1, the size of the surface pores of the SiO decreases from large to small. When the mass ratio of the silicon monoxide to the sodium hydroxide is 3:1, the pore size of the surface is minimal and uniform.
Comparative example 1
Grinding and mixing 5g of silicon monoxide with the particle size of 1-3 mu m in an argon (Ar) filled glove box for 40min; pressing the ground powder into a round sheet with the diameter of 20 mm; putting the slices into a nickel crucible, and heating for 2 hours at 350 ℃ under the argon atmosphere; and crushing the burnt sample, stirring the crushed sample in a conical flask containing deionized water for 12 hours, respectively centrifugally washing the crushed sample for 3 times by using water and ethanol, and finally drying the crushed sample in vacuum at 80 ℃ to obtain the silicon monoxide negative electrode material.
Product detection:
taking the silicon monoxide negative electrode materials of the examples 1-3 and the comparative example 1 respectively, and mixing the silicon monoxide negative electrode material, the acetylene black conductive agent and the CMC binder according to the mass ratio of 7:2:1 stirring and mixing to prepare slurry, coating the slurry on a copper foil, blanking to serve as a negative electrode, taking a lithium sheet as a positive electrode, and taking LiPF as electrolyte solute 6 The solvent is a mixed solution of ethylene carbonate, dimethyl carbonate and ethyl methyl carbonate (the volume ratio of the three is 1. The battery was tested using a battery charge and discharge tester. The results of the battery performance test are shown in table 1, and the battery cycle performance graph is shown in fig. 5.
TABLE 1 results of cell performance test of examples 1-3 and comparative example 1
As can be seen from Table 1, the porous silicon monoxide negative electrode material prepared by the invention has good cycle performance when used as a lithium ion battery negative electrode material. Compared with comparative example 1, the capacity of the porous SiO negative electrode materials prepared in examples 1-3 was higher than that of comparative example 1 after 50 cycles. The porous silicon oxide particles have more pores on the surface, and can well relieve volume expansion generated in the lithium intercalation process, thereby prolonging the cycle life.
Claims (8)
1. A preparation method of porous silicon monoxide cathode material for lithium ion battery is characterized in that silicon monoxide and sodium hydroxide are mixed and then pressed into sheet shape to obtain sheet composite material; carrying out heat treatment on the flaky composite material to obtain a product; crushing the product, stirring in deionized water, washing with alcohol, and drying to obtain the porous silicon monoxide negative electrode material for the lithium ion battery;
the heat treatment temperature is 350-400 ℃, and the heat treatment time is 2-2.5h;
the preparation method of the porous silicon monoxide negative electrode material for the lithium ion battery comprises the following steps:
(1) Grinding sodium hydroxide in inert atmosphere, and sieving;
(2) Grinding and mixing the sodium hydroxide obtained in the step (1) and silicon monoxide in an inert atmosphere to obtain silicon monoxide/sodium hydroxide mixed powder;
(3) Pressing the silicon monoxide/sodium hydroxide mixed powder obtained in the step (2) into a sheet shape to obtain a sheet-shaped composite material;
(4) And (4) carrying out heat treatment on the sheet composite material obtained in the step (3) in an inert atmosphere to obtain a product, crushing the product, stirring the crushed product in deionized water, washing the product with alcohol, and drying the product to obtain the porous silicon monoxide negative electrode material for the lithium ion battery.
2. The preparation method of the porous silicon monoxide negative electrode material for the lithium ion battery as claimed in claim 1, wherein the mass ratio of silicon monoxide to sodium hydroxide is 1.5-3:1.
3. The method for preparing a porous SiO negative electrode material for Li-ion battery according to claim 1, wherein the SiO particle size is 1-3 μm and the mesh size of NaOH is 300-600 mesh.
4. The preparation method of the porous silicon monoxide negative electrode material for the lithium ion battery according to claim 1, wherein the mixing time is 40-60min.
5. The preparation method of the porous silicon monoxide negative electrode material for the lithium ion battery according to claim 1, wherein the sheet shape is a circular sheet shape, and the diameter of the sheet composite material is 20-30mm.
6. The preparation method of the porous silicon monoxide negative electrode material for the lithium ion battery according to claim 1, characterized in that the stirring time is 12-20h.
7. The preparation method of the porous silicon monoxide negative electrode material for the lithium ion battery according to claim 1, wherein the number of washing with water is 3-5, and the number of washing with alcohol is 3-5.
8. The preparation method of the porous silicon monoxide negative electrode material for the lithium ion battery according to claim 1, wherein the drying is vacuum drying, and the drying temperature is 80-100 ℃.
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GB827383A (en) * | 1956-05-25 | 1960-02-03 | Pennsylvania Salt Mfg Co | Production of anhydrous sodium metasilicate |
CN101696033B (en) * | 2009-10-23 | 2011-05-04 | 山东理工大学 | Preparation method for synthesizing sheeted zirconia by using hydrothermal method |
CN102447112B (en) * | 2011-11-30 | 2014-07-30 | 奇瑞汽车股份有限公司 | Silicon-carbon composite material, preparation method thereof and cathode material containing same as well as lithium ion battery |
EP2693533B1 (en) * | 2012-08-03 | 2018-06-13 | LG Chem, Ltd. | Electrode active material for secondary battery |
JP6084856B2 (en) * | 2012-08-22 | 2017-02-22 | 積水化学工業株式会社 | Method for producing carbon material, method for producing electrode material, and method for producing lithium ion secondary battery |
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CN103199227B (en) * | 2013-04-26 | 2015-06-03 | 中国东方电气集团有限公司 | C/Si composite negative nanomaterial of lithium ion battery and preparation method of nanomaterial |
CN103280560B (en) * | 2013-05-20 | 2015-11-11 | 北京科技大学 | The preparation method of the sub-silicon-carbon composite cathode material of the mesoporous oxidation of a kind of lithium ion battery |
CN103413922B (en) * | 2013-08-14 | 2016-08-17 | 湖北万润新能源科技发展有限公司 | The preparation method of lithium ion battery negative material |
CN104617272B (en) * | 2015-02-03 | 2017-10-20 | 东莞市迈科科技有限公司 | A kind of preparation method of porous Si-C composite material |
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