CN116873937A - Method for preparing silica powder by low-temperature solid-phase method - Google Patents
Method for preparing silica powder by low-temperature solid-phase method Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 239000000843 powder Substances 0.000 title claims abstract description 45
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000010532 solid phase synthesis reaction Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 229910021338 magnesium silicide Inorganic materials 0.000 claims abstract description 21
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 238000005554 pickling Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims 1
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 30
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 16
- 239000012265 solid product Substances 0.000 abstract description 16
- 238000002360 preparation method Methods 0.000 abstract description 15
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 13
- 239000007773 negative electrode material Substances 0.000 abstract description 7
- 229910004298 SiO 2 Inorganic materials 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 4
- YJSAVIWBELEHDD-UHFFFAOYSA-N [Li].[Si]=O Chemical compound [Li].[Si]=O YJSAVIWBELEHDD-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 abstract 1
- 239000000956 alloy Substances 0.000 abstract 1
- 229910052744 lithium Inorganic materials 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 239000011889 copper foil Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000006245 Carbon black Super-P Substances 0.000 description 3
- 229910013870 LiPF 6 Inorganic materials 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
- 239000010405 anode material Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000011268 mixed slurry Substances 0.000 description 3
- 239000004584 polyacrylic acid Substances 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000006138 lithiation reaction Methods 0.000 description 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
-
- 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
-
- 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
- H01M4/36—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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Silicon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the field of preparation and application of lithium ion battery materials, and relates to a novel method for preparing silica powder by a low-temperature solid-phase method. The preparation of the silica powder is to prepare magnesium silicide and cheap SiO 2 As raw materials, under the protection of inert gas, magnesium silicide and SiO 2 Mixing in proportion, and reacting for a certain time after the temperature is programmed to the target temperature. And after the reaction is finished, taking out the solid product, and carrying out post-treatment such as acid washing, solid-liquid separation, washing, drying and the like to obtain the silica powder. The method has the advantages of simple preparation process, low cost, mild reaction condition, no environmental pollution and easy realization of industrial production, and provides a new idea for preparing the negative electrode material of the silicon oxide lithium ion battery at low temperature, and the prepared silicon oxide material has excellent electrochemical performance of 0.2A/gThe alloy still has the capacity of 800mAh/g after 50 cycles, the specific capacity and the cycle performance are good, and the method has wide market application prospect.
Description
Technical Field
The invention relates to a method for preparing silicon oxide powder by a low-temperature solid phase and application of the silicon oxide powder as a lithium ion battery negative electrode material, and belongs to the field of preparation and application of lithium ion battery materials.
Background
Today, the application requirements of portable electronic devices and long range electric vehicles have stimulated the rapid development of high specific capacity lithium ion batteries. Among various lithium ion battery anode materials, silicon anode materials have high theoretical capacity (4200 mAh/g) and relatively low oxidation-reduction potential<0.5V vs.Li/Li + ). However, silicon anodes have low conductivity, and have large volume expansion and short battery life during cycling, greatly limiting commercial applications of silicon anodes. Silicon oxide (SiO) is considered as the silicon-based negative electrode material most likely to realize large-scale commercial application because of its abundant reserves, low cost, and easy synthesis. Silicon oxide exhibits less volume change during cycling than silicon cathodes. Li generated in situ during the first lithiation 2 O and lithium silicate can buffer larger volume change, and improve the circulation stability, so that the demand for silicon oxide in the field is growing. The main preparation method of the silicon oxide at present is SiO at high temperature of 1700 DEG C 2 Reacting with simple substance Si to generate gaseous silicon oxide, and rapidly cooling. The method has low yield and high energy consumption, and is not suitable for large-scale industrial production. Therefore, it is of great importance to explore a preparation method of silicon oxide which is efficient, economical, safe, environment-friendly and easy for industrial production.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a novel method for preparing the negative electrode material of the silicon oxide lithium ion battery, which is efficient, low in cost, environment-friendly and easy for industrial production.
In order to achieve the above object, the present invention provides the following technical solutions:
a method for preparing silicon oxide powder by a low-temperature solid-phase method comprises the step of reacting magnesium silicide with silicon dioxide under the protection of inert gas to prepare the silicon oxide.
Preferably, the method specifically comprises the following steps:
(1) Under the protection of inert gas, uniformly mixing magnesium silicide powder and silicon dioxide powder according to a certain proportion to obtain a mixture;
(2) Heating the mixture to a certain temperature under the protection of inert gas to perform chemical reaction;
(3) And after the reaction is finished, carrying out post-treatment on the solid to obtain the silica powder.
Preferably, the magnesium silicide and silicon dioxide SiO in the step (1) 2 The molar ratio of the materials is 1:1-4. By adopting the materials with the proportion for reaction, the magnesium silicide can be further ensured to fully react, and meanwhile, the silicon dioxide is also an excellent lithium battery negative electrode material, so that the silicon dioxide can be directly applied to the lithium battery negative electrode material without separation, and the subsequent processing steps are further simplified.
Preferably, the magnesium silicide powder in the step (1) is in micron order, the particle size is preferably 10-50 microns, and the purity is preferably not less than 99%; more preferably, the silica powder is nano-sized, the particle diameter is preferably 50 to 200nm, and the purity is preferably not less than 95%. The smaller the particle size of the reactant, the higher the purity, the faster the chemical reaction rate, and the more complete the reaction.
Preferably, in the step (1), the substances are uniformly mixed by grinding, so as to be more beneficial to the subsequent reaction.
Preferably, the inert gas in the step (2) is a gas which does not participate in the reaction and does not react, and more preferably at least one of nitrogen, helium and argon.
Preferably, the mixture in the step (2) is placed in a porcelain boat, the porcelain boat is placed in a tube furnace, and the reaction is carried out under the protection of inert gas.
Preferably, the reaction temperature in the step (2) is 550-900 ℃, more preferably the heating rate is 5-10 ℃/min, and the heating is more uniform; more preferably, the reaction time is 3 to 6 hours to substantially complete the reaction, and the reaction time may be appropriately prolonged to make the reaction more complete or shortened to integrate the balance of energy and yield and the like.
Preferably, the post-treatment in the step (3) comprises conventional treatment operations such as acid washing, solid-liquid separation, solid washing, drying and the like; more preferably, the pickling is carried out by using dilute hydrochloric acid to carry out pickling soaking, impurities such as magnesium silicide, magnesium oxide and the like in the solid are further removed, the concentration of the dilute hydrochloric acid is more preferably 1mol/L, the pickling time is preferably 8-15h, and more preferably 10-12h; the solid-liquid separation is preferably filtration, and is a conventional filtration mode such as suction filtration, normal pressure filtration and the like; washing the solid after solid-liquid separation to be neutral by using water; the drying is conventional, more preferably at a temperature of 80-120℃for a period of 10-24 hours.
Preferably, the reaction equation of the method is: mg of 2 Si+3SiO 2 →4SiO+2MgO。
The new method for preparing the silicon oxide powder by the low-temperature solid phase method is to use magnesium silicide and cheap SiO 2 As raw materials, magnesium silicide and SiO are protected by inert gas such as Ar gas 2 The gases are mixed according to a certain proportion and placed in a tube furnace, the temperature programming is started under the condition of room temperature, and the reaction is carried out for a certain time after the temperature is raised to 550-900 ℃ at a certain temperature raising rate. And after the reaction is finished, taking out the solid product, soaking the solid product with an acidic substance, carrying out solid-liquid separation, washing and drying to obtain the silicon oxide anode material. The preparation method provided by the invention has the advantages of simple process, low cost, no environmental pollution and easiness in realizing industrialized mass production, and provides a new thought for preparing the negative electrode material of the silicon oxide lithium ion battery at low temperature for the field, and the prepared silicon oxide material has excellent electrochemical performance and still has 800mAh/g capacity after 50 cycles of 0.2A/g.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention utilizes magnesium silicide and SiO 2 The reaction is carried out under the protection of inert gas to generate the silicon oxide, the process can be carried out at a lower temperature, and the blank of the technology for synthesizing the silicon oxide powder at a low temperature by a solid phase method is made up;
(2) The preparation method has the advantages of simple preparation process, wide and easily available raw material sources, low cost, high efficiency, mild reaction conditions, environmental protection and easy industrialized mass production implementation;
(3) The silicon oxide material prepared by the invention has excellent electrochemical performance, and after 50 cycles, 0.2A/g still has 800mAh/g capacity, and the specific capacity and the cycle performance are both good, so that the silicon oxide material has wide market application prospect.
Drawings
FIG. 1 is an X-ray diffraction pattern (XRD) of the silica powder prepared in example 1;
FIG. 2 is a Scanning Electron Micrograph (SEM) of the silica prepared according to example 1;
fig. 3 is a graph of the cycling performance of the simulated lithium ion battery prepared in example 1.
Detailed Description
The technical solution of the present invention will be further clearly and completely described below by means of specific examples, and with reference to the accompanying drawings, it should be understood that the described examples of the present invention are implemented on the premise of the technical solution of the present invention, and detailed implementation and specific operation procedures are given, but only some examples of the present invention are not all examples. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The experimental methods used in the following examples are conventional methods unless otherwise specified, and the materials, reagents, etc. used in the examples are commercially available unless otherwise specified.
Example 1:
the first step: preparation of silica powder
The magnesium silicide powder and the silicon dioxide powder were stored in a glove box. Under the protection of argon atmosphere, 0.17g of magnesium silicide and 0.4g of SiO are firstly added 2 The powder is ground and mixed, placed in a porcelain boat and placed in a tube furnace. And (3) introducing Ar gas for 30min for gas replacement and evacuation, then heating the furnace tube to 650 ℃ at a heating rate of 5 ℃/min, and carrying out heat preservation reaction for 6h. After the reaction is finished, taking out the solid product, soaking the solid product in 1mol/L dilute hydrochloric acid for 10 hours, filtering the solid product, and washing the solid product with deionized water until the solution is neutral. Drying at 80 ℃ for 12 hours, and cooling to obtain 0.36g of powder, namely the silicon oxide, wherein the yield is 91%, and the purity of the silicon oxide is higher than 99%.
FIG. 1 is an X-ray diffraction pattern (XRD) of the silica powder prepared in this example, wherein a is the XRD pattern of the solid product before acid washing, b is the XRD pattern of the final product after acid washing, and c is the XRD pattern of commercial SiO; fig. 2 is a Scanning Electron Micrograph (SEM) of the silica prepared in example 1, which shows that the silica prepared is in the form of microspheres with a particle size of less than 5 microns.
And a second step of: preparation of simulated lithium ion battery
Silica powder, super-P and 25% polyacrylic acid aqueous solution are respectively weighed according to the mass ratio of 6:2:2, deionized water is used as a solvent, and the mixture is magnetically stirred to form slurry with uniform components and moderate viscosity. And (3) coating the uniformly mixed slurry on a copper foil, and drying the copper foil in a vacuum oven at 120 ℃ for more than 8 hours to obtain the electrode plate. The lithium metal sheet is used as a counter electrode, and the electrolyte is 1mol/L LiPF 6 And (3) an EC-DMC (1:1) solution, wherein a polypropylene microporous film is used as a diaphragm, and the simulated lithium ion battery is assembled. Fig. 3 is a cycle performance chart of the simulated lithium ion battery prepared in the embodiment, and as can be seen from fig. 3, the initial discharge 1850mAh/g still has a capacity of 800mAh/g after 50 cycles, and has better cycle stability; meanwhile, a simulated lithium electronic battery is prepared from a commercial silicon oxide material according to the same method, and fig. 3 shows that the initial discharge of the battery is 2120mAh/g, but the capacity decay is quicker, the capacity is reduced to 420mAh/g after 50 cycles, the capacity retention rate is only 19.8%, and the specific capacity and the cycle performance of the battery prepared from the silicon oxide material are obviously better than those of the commercial silicon oxide material.
Example 2:
the first step: preparing silica powder
The magnesium silicide powder and the silicon dioxide powder were stored in a glove box. Under the protection of argon atmosphere, 0.51g of magnesium silicide and 0.4g of SiO are firstly added 2 The powder is ground and mixed and placed in a tube furnace. After the Ar gas is introduced for 30min for emptying, the temperature of the furnace tube is raised to 900 ℃ at a heating rate of 5 ℃/min, and the temperature is kept for reaction for 3h. After the reaction is finished, taking out the solid product, soaking the solid product in 1mol/L dilute hydrochloric acid for 10 hours, filtering the solid product, and washing the solid product with deionized water until the solution is neutral. Drying in an oven at 120 ℃ for 24 hours, and cooling to obtain powder, namely the silicon oxide.
And a second step of: preparation of simulated lithium ion battery
The simulated lithium electronic battery of this example was prepared according to the preparation method of the simulated lithium electronic battery of example 1, specifically: silica powder, super-P and 25% polyacrylic acid aqueous solution are respectively weighed according to the mass ratio of 6:2:2, deionized water is used as a solvent, and the mixture is magnetically stirred to form slurry with uniform components and moderate viscosity. And uniformly coating the uniformly mixed slurry on a copper foil, and drying the copper foil in a vacuum oven at 120 ℃ for more than 8 hours to obtain the electrode plate. The lithium metal sheet is used as a counter electrode, and the electrolyte is 1mol/L LiPF 6 And (3) an EC-DMC (1:1) solution, wherein a polypropylene microporous film is used as a diaphragm, and the simulated lithium ion battery is assembled. The first-round discharge is 1750mAh/g, the capacity of 920mAh/g is still provided after 50 circles of circulation, has better circulation stability.
Example 3:
the first step: preparing silica powder
The magnesium silicide powder and the silicon dioxide powder were stored in a glove box. Under the protection of argon atmosphere, 0.34g of magnesium silicide and 0.4g of SiO are firstly added 2 The powder is ground and mixed and placed in a tube furnace. And (3) introducing Ar gas for 30min for emptying, then heating the furnace tube to 550 ℃ at a heating rate of 10 ℃/min, and carrying out heat preservation reaction for 6h. After the reaction is finished, taking out the solid product, soaking the solid product in 1mol/L dilute hydrochloric acid for 12 hours, filtering the solid product, and washing the solid product with deionized water until the solution is neutral. Drying in oven at 120deg.C for 24 hr, coolingThe powder obtained is silica.
And a second step of: preparation of simulated lithium ion battery
The simulated lithium electronic battery of this example was prepared according to the preparation method of the simulated lithium electronic battery of example 1, specifically: silica powder, super-P and 25% polyacrylic acid aqueous solution are respectively weighed according to the mass ratio of 6:2:2, deionized water is used as a solvent, and the mixture is magnetically stirred to form slurry with uniform components and moderate viscosity. And uniformly coating the uniformly mixed slurry on a copper foil, and drying the copper foil in a vacuum oven at 120 ℃ for more than 8 hours to obtain the electrode plate. The lithium metal sheet is used as a counter electrode, and the electrolyte is 1mol/L LiPF 6 And (3) an EC-DMC (1:1) solution, wherein a polypropylene microporous film is used as a diaphragm, and the simulated lithium ion battery is assembled. The initial charge of 1810mAh/g is that after 50 circles of circulation, the capacity of 1025mAh/g is still provided, and the circulation stability is better.
The above only shows the preferred embodiments of the present invention, the scope of the present invention is not limited thereto, and any changes made by those skilled in the art within the scope of the claims of the present invention fall within the scope of the present invention.
Claims (10)
1. A method for preparing silica powder by a low-temperature solid-phase method is characterized in that magnesium silicide and silicon dioxide are reacted under the protection of inert gas to prepare the silica.
2. A method for preparing silica powder by a low temperature solid phase method according to claim 1, wherein the method specifically comprises the following steps:
(1) Under the protection of inert gas, uniformly mixing magnesium silicide powder and silicon dioxide powder according to a certain proportion to obtain a mixture;
(2) Heating the mixture to a certain temperature under the protection of inert gas to perform chemical reaction;
(3) And after the reaction is finished, carrying out post-treatment on the solid to obtain the silica powder.
3. According toThe method for preparing silica powder by a low temperature solid phase method according to claim 2, wherein the magnesium silicide and the silica SiO in the step (1) are 2 The molar ratio of the materials is 1:1-4.
4. The method for preparing silica powder by a low temperature solid phase method according to claim 2, wherein the magnesium silicide powder in the step (1) is in a micrometer scale and the silica powder is in a nanometer scale.
5. A method for preparing silica powder by a low temperature solid phase method as claimed in claim 2, wherein the reaction temperature in the step (2) is 550 to 900 ℃.
6. A method for preparing silica powder by a low temperature solid phase method as claimed in claim 5, wherein the temperature rising rate in the step (2) is 5-10 ℃.
7. A method for preparing silica powder by a low temperature solid phase method as claimed in claim 5, wherein the reaction time in the step (2) is 3 to 6 hours.
8. A method for preparing silica powder by a low temperature solid phase method according to claim 1, wherein the post-treatment in the step (3) comprises acid washing, solid-liquid separation, solid washing, and drying.
9. The method for preparing the silica powder by the low-temperature solid phase method according to claim 8, wherein the pickling is to carry out pickling soaking by using dilute hydrochloric acid, the concentration of the dilute hydrochloric acid is 1mol/L, and the pickling time is 8-15 hours; drying at 80-120deg.C for 10-24 hr.
10. A method for preparing silica powder by a low temperature solid phase method according to claim 1, wherein the reaction equation of the method is: mg of 2 Si+3SiO 2 →4SiO+2MgO。
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310716421.3A CN116873937A (en) | 2023-06-16 | 2023-06-16 | Method for preparing silica powder by low-temperature solid-phase method |
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| CN202310716421.3A CN116873937A (en) | 2023-06-16 | 2023-06-16 | Method for preparing silica powder by low-temperature solid-phase method |
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| CN110676444A (en) * | 2019-08-26 | 2020-01-10 | 浙江工业大学 | Method for preparing silicon/carbon nanotube composite material in situ by one-pot method |
| CN112331854A (en) * | 2020-10-30 | 2021-02-05 | 浙江锂宸新材料科技有限公司 | Lithium magnesium silicate pre-lithiated silicon monoxide negative electrode material and preparation method and application thereof |
| CN113054180A (en) * | 2021-03-24 | 2021-06-29 | 浙江锂宸新材料科技有限公司 | Graphite @ silicon carbide @ silicon negative electrode material and preparation method and application thereof |
| CN115893420A (en) * | 2022-09-19 | 2023-04-04 | 华宇新能源科技有限公司 | Hollow three-dimensional porous silicon material and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110676444A (en) * | 2019-08-26 | 2020-01-10 | 浙江工业大学 | Method for preparing silicon/carbon nanotube composite material in situ by one-pot method |
| CN112331854A (en) * | 2020-10-30 | 2021-02-05 | 浙江锂宸新材料科技有限公司 | Lithium magnesium silicate pre-lithiated silicon monoxide negative electrode material and preparation method and application thereof |
| CN113054180A (en) * | 2021-03-24 | 2021-06-29 | 浙江锂宸新材料科技有限公司 | Graphite @ silicon carbide @ silicon negative electrode material and preparation method and application thereof |
| CN115893420A (en) * | 2022-09-19 | 2023-04-04 | 华宇新能源科技有限公司 | Hollow three-dimensional porous silicon material and preparation method thereof |
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