CN112436131B - Method for preparing silicon-carbon composite material by molten salt assisted magnesiothermic reduction - Google Patents

Method for preparing silicon-carbon composite material by molten salt assisted magnesiothermic reduction Download PDF

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CN112436131B
CN112436131B CN202011426521.5A CN202011426521A CN112436131B CN 112436131 B CN112436131 B CN 112436131B CN 202011426521 A CN202011426521 A CN 202011426521A CN 112436131 B CN112436131 B CN 112436131B
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composite material
molten salt
silicon
attapulgite
carbon composite
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CN112436131A (en
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周小中
田继斌
祁赵一
刘强
费莎莎
鲁鸿凯
丁娟霞
雷自强
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Northwest Normal University
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    • 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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention provides a method for preparing a silicon-carbon composite material by using molten salt to assist magnesiothermic reduction, which comprises the steps of firstly carbonizing alginate and attapulgite serving as raw materials at high temperature to obtain an amorphous carbon coating-coated attapulgite composite material, then adding a reducing agent and molten salt to perform heat-assisted reduction reaction, and performing acid pickling treatment to obtain the silicon-carbon composite material. The invention realizes the method for preparing the silicon-carbon composite material by combining high-temperature carbonization and low-temperature molten salt heat assistance, effectively reduces the generation of silicon carbide through the molten salt heat assistance reduction reaction, and the carbon coating in the prepared silicon-carbon composite material coats silicon nano particles reduced by attapulgite and forms a gap structure through acid etching. The composite material is used for a lithium ion battery cathode material, and the carbon layer, the gaps and the porous structure can effectively relieve the volume expansion effect caused in the lithium intercalation and deintercalation process, and simultaneously improve the electronic conductivity, so that the composite material has excellent electrochemical lithium storage performance.

Description

Method for preparing silicon-carbon composite material by molten salt assisted magnesiothermic reduction
Technical Field
The invention relates to a method for preparing a silicon-carbon composite material by using molten salt to assist magnesiothermic reduction, which is mainly used for a lithium ion battery cathode material and belongs to the technical field of composite materials and the technical field of new energy.
Background
The endurance of new energy automobiles and electronic products depends on the energy density of the battery, and with the continuous improvement of consumer demand, the automobiles and electronic products with long endurance are deeply liked by consumers. Therefore, the search for high energy density batteries will be the direction and power of future development. Of all the materials that can fulfill this need, silicon-based materials are one of the most promising candidates due to their high theoretical capacity (Si, 4200 mAh g) -1 ) Low operating potential, wide source and the like, so that the material becomes a high-hotspot material in application research. However, the silicon negative electrode material generates huge volume expansion (300%) and serious interface side reaction in the lithium intercalation and lithium deintercalation processes, which are key problems that further stable application of high energy density is prevented, and the problems can be solved to the greatest extent by reasonably designing the structure of the silicon negative electrode material and coating of a carbon layer. Meanwhile, the method is also important for the selection of a silicon source and a carbon source, and the research on the preparation and the application of the method is very important.
Attapulgite, also called attapulgite, is a natural inorganic material with wide source and low cost, and the ideal chemical component is Mg 5 Si 8 O 20 (OH) 2 (H 2 O) 4 .nH 2 O, wherein SiO 2 The content is about 57 percent, and SiO in the pretreated attapulgite 2 The content can be improved to more than 65 percent, and the silicon nano material obtained by reducing the silicon nano material serving as a silicon source has wide application prospect and practical significance. Alginate is a pure natural polysaccharide and is a high-viscosity polymer compound. Because the silicon anode material has high-strength viscosity, the silicon anode material is selected as a carbon source to more easily realize the coating effect of a carbon coating, so that the silicon anode material has excellent specific capacity and long cycle service life. Therefore, the application of the attapulgite in the aspect of silicon-based anode materials has profound influence, great application prospect and economic and commercial values.
The invention patent (publication number: CN 109873150A) discloses a method for directly reducing palygorskite into silicon nano-particles at high temperature and then compounding the silicon nano-particles with carbon source graphene to obtain a silicon-carbon composite material. The reduction temperature used in the patent is high, the process is complex, and the preparation process comprises the steps of firstly obtaining a silicon simple substance by high-temperature reduction and then carrying out carbonization coating on the silicon simple substance to prepare the silicon-carbon composite material.
Disclosure of Invention
The invention aims to provide a method for preparing a silicon-carbon composite material by using molten salt to assist magnesiothermic reduction.
1. Preparation of silicon-carbon composite material
The method for preparing the silicon-carbon composite material by using the molten salt to assist the magnesiothermic reduction comprises the following steps of:
(1) Pretreating attapulgite, uniformly dispersing in an ethanol-water mixed solution to obtain an attapulgite dispersion liquid, dissolving alginate in deionized water to obtain an alginate solution, uniformly mixing the attapulgite dispersion liquid and the alginate solution, stirring to dry, and carbonizing at high temperature under the protection of inert gas to obtain the amorphous carbon coating-coated attapulgite composite material. Wherein the attapulgite is pretreated by drying and dewatering the attapulgite at 100-300 ℃, and then washing with HCl with the concentration of 2-10 mol/L. In the ethanol-water mixed solution, the volume ratio of ethanol to water is 1. The alginate is potassium alginate or sodium alginate. The mass ratio of the alginate to the attapulgite is 1 to 1. The high-temperature carbonization temperature is 700-1000 ℃, and the high-temperature carbonization time is 1-5h.
(2) Mixing the amorphous carbon coating coated attapulgite composite material, reducing agent magnesium powder and molten salt, reacting for 2-8h at 650-850 ℃ under the protection of inert gas, cooling to room temperature, washing with hydrochloric acid and hydrofluoric acid, washing with deionized water and absolute ethyl alcohol, and drying to obtain the silicon-carbon composite material. Wherein the mass ratio of the attapulgite composite material coated with the amorphous carbon coating to the magnesium powder serving as the reducing agent is 1 to 1. The molten salt is sodium chloride or potassium chloride, and the mass ratio of the amorphous carbon coating-coated attapulgite composite material to the molten salt is (1).
2. Structural characterization of silicon carbon composites
The structure of the silicon-carbon composite material prepared by the invention is characterized by an X-ray diffraction pattern (XRD) and a Scanning Electron Microscope (SEM).
FIG. 1 is an X-ray diffraction pattern (XRD) of a silicon carbon composite material prepared according to the present invention. It can be seen from fig. 1 that the diffraction peaks of the silicon-carbon composite materials prepared in examples 1 and 2 completely match with the strong diffraction peaks of the elemental Si phase (JCPDS card number 27-1402), indicating that the silicon-carbon composite material was successfully synthesized, and it can be seen from the figure that the material prepared in example 2 contains a large amount of impurity silicon carbide, indicating that the reduction temperature is increased and the content of the impurity silicon carbide is increased.
Fig. 2 is a Scanning Electron Microscope (SEM) image of the silicon carbon composite material prepared by the present invention. The morphology of the silicon-carbon composite materials prepared in examples 1 and 2 can be seen from fig. 2, and it can be seen from both figures that the reduced silicon nanoparticles are coated in the carbon layer and agglomerated into a large block, and the void-groove structure formed by acid etching can also be seen. The particles in example 1 were found to be smaller than those in example 2 by comparison, indicating that an increase in the reduction temperature would result in an increase in the sample particles.
3. Performance test of silicon-carbon composite material as lithium ion battery cathode material
The test method comprises the following steps: grinding a certain amount of silicon-carbon composite material, sodium alginate and acetylene black to prepare slurry, assembling the slurry into a button cell, and testing the cycle performance of the button cell by adopting a blue test system.
FIG. 3 is a cycle performance diagram of the silicon-carbon composite material prepared by the invention as a lithium ion battery cathode. It can be seen from FIG. 3 that the silicon-carbon composite materials prepared in examples 1 and 2 are 200mA g in the case of being used as the negative electrode material of a lithium ion battery -1 Respectively has 1221.1 mAh g at a current density of -1 、1352.8 mAh g -1 The initial reversible specific capacity is 68.66 percent and 59.38 percent respectively. After 100 cycles, the reversible specific capacity is respectively kept at 731.3 mAh g -1 And 514.7 mAh g -1 The silicon-carbon composite material prepared by the invention has good cycling stability.
In conclusion, the invention uses alginate and attapulgite as raw materials, firstly carries out high-temperature carbonization to obtain the amorphous carbon coating coated attapulgite composite material, then adds a reducing agent and molten salt to carry out heat-assisted reduction reaction, and carries out acid pickling treatment to obtain the silicon-carbon composite material. The invention realizes the method for preparing the silicon-carbon composite material by combining high-temperature carbonization and low-temperature molten salt heat assistance, effectively reduces the generation of silicon carbide through the molten salt heat assistance reduction reaction, and the carbon coating in the prepared silicon-carbon composite material coats silicon nano particles reduced by attapulgite and forms a gap structure through acid etching. The composite material is used for a lithium ion battery cathode material, and the carbon layer, the gaps and the porous structure can effectively relieve the volume expansion effect caused in the lithium intercalation and deintercalation process, and simultaneously improve the electronic conductivity, so that the composite material has excellent electrochemical lithium storage performance.
Drawings
FIG. 1 is an X-ray diffraction pattern (XRD) of a silicon carbon composite material prepared according to various embodiments of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) image of a silicon carbon composite material prepared according to various embodiments of the present invention;
fig. 3 is a graph of cycle performance of the silicon-carbon composite material prepared in different embodiments of the present invention as a negative electrode of a lithium ion battery.
Detailed Description
The preparation and properties of the silicon-carbon composite material of the present invention are described in detail by the following specific examples.
Example 1
(1) Firstly drying attapulgite at 200 deg.C to remove water, washing with 4mol/L HCl solution, and uniformly dispersing 2g pretreated attapulgite in 300mL ethanol-water mixed solution (V) Ethanol : V Water (W) = 1); dissolving 2g of sodium alginate in 100ml of deionized water to form a sodium alginate solution; mixing and stirring the attapulgite dispersion liquid and the sodium alginate solution, and carbonizing at 800 ℃ for 5 hours under the protection of inert gas to obtain the amorphous carbon coating-coated attapulgite composite material.
(2) Mixing the amorphous carbon coating coated attapulgite composite material with magnesium powder according to the mass ratio of 1.
The composite material is used as lithium ionWhen the battery cathode material is used, the current is 200mA g -1 Has a current density of 1221.1 mAh g -1 The initial reversible specific capacity of the catalyst is high, and the initial coulombic efficiency is 68.66 percent. After 100 cycles, the product can maintain 731.3 mAh g -1 Has excellent cycle stability.
Example 2
(1) Firstly drying attapulgite at 300 deg.C to remove water, washing with 8mol/L HCl solution, and uniformly dispersing 4g pretreated attapulgite in 300mL ethanol-water mixed solution (V) Ethanol : V Water (W) = 1); dissolving 2g of potassium alginate in 100ml of deionized water to form a potassium alginate solution; mixing and stirring the attapulgite dispersion liquid and the potassium alginate solution, and carbonizing at 900 ℃ for 2h under the protection of inert gas to obtain the amorphous carbon coating-coated attapulgite composite material.
(2) Mixing the amorphous carbon coating coated attapulgite composite material with magnesium powder according to the mass ratio of 1.
When the composite material is used as a negative electrode material of a lithium ion battery, the concentration of the composite material is 200mA g -1 Has a current density of 1352.8 mAh g -1 The first coulombic efficiency was 59.38%. After 100 cycles, 514.7 mAh g can be maintained -1 Has good cycle stability.

Claims (8)

1. A method for preparing a silicon-carbon composite material by molten salt assisted magnesiothermic reduction comprises the following steps:
(1) Pretreating attapulgite, uniformly dispersing in an ethanol-water mixed solution to obtain an attapulgite dispersion liquid, dissolving alginate in deionized water to obtain an alginate solution, mixing the attapulgite dispersion liquid and the alginate solution, stirring, and carbonizing at high temperature under the protection of inert gas to obtain an amorphous carbon coating coated attapulgite composite material; the high-temperature carbonization temperature is 700-1000 ℃, and the high-temperature carbonization time is 1-5h;
(2) Mixing the amorphous carbon coating coated attapulgite composite material, reducing agent magnesium powder and molten salt, reacting for 2-8h at 650-850 ℃ under the protection of inert gas, cooling to room temperature, washing with hydrochloric acid and hydrofluoric acid, washing with deionized water and absolute ethyl alcohol, and drying to obtain the silicon-carbon composite material.
2. The method for preparing the silicon-carbon composite material by the molten salt assisted magnesium thermal reduction according to claim 1, wherein the molten salt assisted magnesium thermal reduction comprises the following steps: in the step (1), the attapulgite is pretreated by drying and dewatering the attapulgite at 100-300 ℃, and then washing the attapulgite with HCl with the concentration of 2-10 mol/L.
3. The method for preparing the silicon-carbon composite material by the molten salt assisted magnesium thermal reduction according to claim 1, wherein the molten salt assisted magnesium thermal reduction comprises the following steps: in the step (1), in the ethanol-water mixed solution, the volume ratio of ethanol to water is 1.
4. The method for preparing the silicon-carbon composite material by the molten salt assisted magnesiothermal reduction according to claim 1, wherein the molten salt assisted magnesiothermal reduction comprises the following steps: in the step (1), the alginate is potassium alginate or sodium alginate.
5. The method for preparing the silicon-carbon composite material by the molten salt assisted magnesium thermal reduction according to claim 1, wherein the molten salt assisted magnesium thermal reduction comprises the following steps: in the step (1), the mass ratio of the alginate to the attapulgite is 1 to 1.
6. The method for preparing the silicon-carbon composite material by the molten salt assisted magnesium thermal reduction according to claim 1, wherein the molten salt assisted magnesium thermal reduction comprises the following steps: in the step (2), the mass ratio of the amorphous carbon coating coated attapulgite composite material to the reducing agent magnesium powder is 1 to 1.
7. The method for preparing the silicon-carbon composite material by the molten salt assisted magnesiothermal reduction according to claim 1, wherein the molten salt assisted magnesiothermal reduction comprises the following steps: in the step (2), the molten salt is sodium chloride or potassium chloride, and the mass ratio of the amorphous carbon coating-coated attapulgite composite material to the molten salt is (1) - (10) - (1).
8. The silicon-carbon composite material prepared by the method of claim 1 is applied to a lithium ion battery cathode material.
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CN113998702B (en) * 2021-10-13 2023-10-13 昆明理工大学 Method for preparing Si/C anode material by taking micro silicon powder as raw material
CN115353118A (en) * 2022-09-23 2022-11-18 淮阴工学院 Method for modifying attapulgite clay by molten salt

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