CN111540892A - Preparation method of iron-based-carbon composite material with core-shell structure - Google Patents

Preparation method of iron-based-carbon composite material with core-shell structure Download PDF

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CN111540892A
CN111540892A CN202010395414.4A CN202010395414A CN111540892A CN 111540892 A CN111540892 A CN 111540892A CN 202010395414 A CN202010395414 A CN 202010395414A CN 111540892 A CN111540892 A CN 111540892A
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iron
core
carbon composite
composite material
shell structure
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CN111540892B (en
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高敏
孙磊
邹文珍
张林浩
梁攀飞
曹江行
范美强
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China Jiliang 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
    • 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
    • H01M4/58—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
    • 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
    • H01M4/582—Halogenides
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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 discloses a preparation method of an iron-based-carbon composite material with a core-shell structure, which comprises the steps of taking soluble ferric salt as a raw material, performing ferric salt hydrothermal reaction, tetraethyl silicate hydrolysis and polymer coating, repeating the cycle for 0-3 times, treating with strong alkali, carbonizing, and finally reacting with iodine to obtain the iron-based-carbon composite material with the core-shell structure; the iron-based-carbon composite material is of a micro-nano structure and contains 1-4 layers of core-shell structures; the iron-based-carbon composite material has good electrochemical performance and good application prospect in the field of batteries.

Description

Preparation method of iron-based-carbon composite material with core-shell structure
Technical Field
The invention relates to a preparation method of an electrode material, in particular to a preparation method of an iron-based-carbon composite material with a core-shell structure.
Background
The core-shell material has a double-layer or multi-layer structure, and different components are respectively enriched inside and outside the core-shell material, so that the functions of the core and the shell are compounded and complemented, and a novel functional material with the performance different from that of the core or the shell can be prepared. Designing and constructing a nanocomposite material with a core-shell structure is a leading field of material science in recent years. The core-shell structure material can realize the compounding and complementation of core and shell functions, and the design concept of the core-shell structure is introduced into the lithium ion battery material in recent years. The negative electrode material taking iron ions in various valence states as ligands is widely applied, such as iron metal oxide, iron disulfide and the like, but the capacity attenuation of the negative electrode material is obvious along with the charge and discharge.
Patent CN 109148864A discloses a ferrous disulfide composite cathode material and a preparation method thereof; the conductive polymer layer is coated on the surface of the iron disulfide, so that the conductivity of the iron disulfide is improved, the conductive polymer layer has certain toughness, and the volume expansion of the iron disulfide in the charging and discharging processes can be buffered, so that the cycling stability of the battery is obviously improved.
Patent CN 108736000A discloses a method for preparing Fe by thermal decomposition2O3A method for preparing a carbon nanotube composite material. The mixture of ferric nitrate and carbon nanotubes was calcined in a tube furnace in an inert gas. The Fe2O3The carbon nanotube composite material has good cycle life, coulombic efficiency, and relatively high energy density and cycle stability.
However, the iron-based electrode material has poor conductivity, and how to improve the electrochemical performance of the iron-based electrode material still needs to be solved.
Disclosure of Invention
Aiming at the defects of the prior art scheme, the invention aims to provide a preparation method of an iron-based-carbon composite material with a core-shell structure.
The invention relates to a preparation method of an iron-based-carbon composite material with a core-shell structure, which comprises the steps of taking soluble ferric salt as a raw material, performing ferric salt hydrothermal reaction, tetraethyl silicate hydrolysis and polymer coating, repeating the cycle for 0-3 times, treating with strong alkali, carbonizing, and finally reacting with iodine to obtain the iron-based-carbon composite material with the core-shell structure; the soluble ferric salt is one of ferric chloride, ferric bromide, ferric nitrate and ferric acetate; the polymer precursor is phenol compound and aldehyde compound; the phenol compound is one of phenol, m-diphenol, m-triphenol, p-phenol and o-phenol; the aldehyde compound is one of formaldehyde, acetaldehyde, propionaldehyde and butyraldehyde; a preparation method of an iron-based-carbon composite material with a core-shell structure comprises the following steps:
1) weighing a certain mass of soluble ferric salt, trisodium citrate and an ethanol/water mixture, mixing, and carrying out hydrothermal reaction at 100-240 ℃ for 3-20 hours; wherein the volume ratio of ethanol to water is 80-100;
2) dispersing the product obtained in the step 1 in an alcohol solvent, adding water and tetraethyl silicate, and stirring for 5-10 hours at the temperature of 20-70 ℃; filtering and washing; wherein the molar ratio of iron to silicon is 2-5;
3) sequentially adding the product in the step 2 into hexadecyltrimethylamine bromide, water, a phenol compound, absolute ethyl alcohol, ammonia water and an aldehyde compound, and stirring for 5-10 hours at the temperature of 20-70 ℃; filtering and washing;
4) adding the product of the step 3 into N2Carbonizing at the temperature of 800 ℃ for 2-10h under the atmosphere of 400-;
5) repeating the product of the step 4 for 0-3 times of cycles of the step 1, the step 2, the step 3 and the step 4;
6) putting the product obtained in the step 5 into a strong alkali solution for 5-10 hours; washing and drying;
7) mixing the product obtained in the step 6 with iodine, and carrying out solid solution at the temperature of 100-200 ℃ for 2-10 hours; then solid solution is carried out for 1-5 hours at the temperature of 400-800 ℃; obtaining the iron-based-carbon composite material with the core-shell structure; wherein the molar ratio of iodine to iron is 0.2-1.2; the iron-based-carbon composite material contains 1-4 layers of core-shell structures;
the iron-based-carbon composite material contains micro-nano structures;
the molar ratio of the iron element to the phenol compound is 0.5-5;
the molar ratio of the phenol compound to the aldehyde compound is 1-1.5.
The iron oxide-carbon with a core-shell structure is designed as a raw material, and the iron-based-carbon composite material with the core-shell structure is prepared through an iodine reaction. Compared with the prior art, the preparation method of the iron-based-carbon composite material with the core-shell structure provided by the invention has the following advantages:
1) the preparation process is simple, the working procedures are controllable, and industrial production can be realized;
2) guiding silicon dioxide to deposit on the surface by taking iron oxide as a template, polymerizing a conductive material on the surface, depositing the iron oxide, removing the silicon dioxide, carbonizing, and reacting with iodine to form a micro-nano core-shell structure; the conductivity of the electrode material is greatly improved;
3) the iron-based-carbon composite material with the micro-nano core-shell structure is beneficial to the intercalation/desorption of lithium ions. The specific capacity and the rate capability of the electrode material are greatly improved; the material has good application prospect in the field of lithium ion batteries.
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following embodiments are described in detail as follows:
example 1
A preparation method of an iron-based-carbon composite material with a layer of core-shell structure comprises the following steps:
1) weighing a certain mass of soluble ferric salt, trisodium citrate and an ethanol/water mixture, mixing, and carrying out hydrothermal reaction at 160 ℃ for 10 hours; wherein the volume ratio of ethanol to water is 80;
2) dispersing the product obtained in the step 1 in an alcohol solvent, adding water and tetraethyl silicate, and stirring for 5 hours at 40 ℃; filtering and washing; wherein the molar ratio of iron to silicon is 5;
3) sequentially adding the product in the step 2 into hexadecyltrimethylamine bromide, water, a phenol compound, absolute ethyl alcohol, ammonia water and an aldehyde compound, and stirring for 5 hours at 50 ℃; filtering and washing;
4) adding the product of the step 3 into N2Carbonizing for 5 hours at 600 ℃ in the atmosphere;
5) putting the product obtained in the step 4 into a strong alkali solution for 10 hours; washing and drying;
6) mixing the product obtained in the step 5 with iodine, and performing solid solution at 150 ℃ for 5 hours; then solid dissolving for 2 hours at 500 ℃; obtaining the iron-based-carbon composite material with a layer of core-shell structure.
The component design of the iron-based-carbon composite material with a layer of core-shell structure comprises the following steps:
1)0.1mol of ferric chloride; 0.025mol tetraethyl silicate; 0.25mol of resorcinol; 0.2mol of formaldehyde; 0.06mol of iodine;
2)0.1mol of ferric nitrate; 0.03mol tetraethyl silicate; 0.2mol of phenol; 0.20mol of formaldehyde; 0.08mol of iodine;
microstructure display: the iron-based-carbon composite material has a micro-nano core-shell structure, and the carbon core shell covers the iron-based electrode material; the electrochemical test results show that: the iron-based-carbon composite material has good electrochemical performance.
Example 2
A preparation method of an iron-based-carbon composite material with a two-layer core-shell structure comprises the following steps:
1) weighing a certain mass of soluble ferric salt, trisodium citrate and an ethanol/water mixture, mixing, and carrying out hydrothermal reaction at 180 ℃ for 5 hours; wherein the volume ratio of ethanol to water is 90;
2) dispersing the product obtained in the step 1 in an alcohol solvent, adding water and tetraethyl silicate, and stirring for 5 hours at 40 ℃; filtering and washing; wherein the molar ratio of iron to silicon is 4;
3) sequentially adding the product in the step 2 into hexadecyltrimethylamine bromide, water, a phenol compound, absolute ethyl alcohol, ammonia water and an aldehyde compound, and stirring for 5 hours at 50 ℃; filtering and washing;
4) adding the product of the step 3 into N2Carbonizing for 10h at 500 ℃ in the atmosphere;
5) repeating the cycle of the steps 1,2,3 and 4 for 1 time by using the product obtained in the step 4;
6) putting the product obtained in the step 5) into a strong alkali solution for 10 hours; washing and drying;
7) mixing the product obtained in the step 6 with iodine, and performing solid solution at 200 ℃ for 3 hours; then solid dissolving for 2 hours at 600 ℃; obtaining the iron-based-carbon composite material with a two-layer core-shell structure.
The component design of the iron-based-carbon composite material with the two-layer core-shell structure comprises the following steps:
3) a first layer: 0.025mol ferric chloride; 0.0125mol of tetraethyl silicate; 0.12mol of resorcinol; 0.1mol of formaldehyde; 0.025mol iodine;
a second layer: 0.05mol of ferric chloride; 0.0125mol of tetraethyl silicate; 0.22mol of resorcinol; 0.2mol of formaldehyde; 0.04mol of iodine;
4) a first layer: 0.03mol of ferric bromide; 0.0125mol of tetraethyl silicate; 0.12mol of phloroglucinol; 0.12mol of formaldehyde; 0.02mol of iodine;
a second layer: 0.05mol of ferric bromide; 0.0125mol of tetraethyl silicate; 0.20mol of phloroglucinol; 0.15mol of formaldehyde; 0.04mol of iodine;
microstructure display: the iron-based-carbon composite material has a micro-nano core-shell structure, and the carbon core shell covers the iron-based electrode material; the electrochemical test results show that: the iron-based-carbon composite material has good electrochemical performance.
Example 3
A preparation method of an iron-based-carbon composite material with a three-layer core-shell structure comprises the following steps:
1) weighing a certain mass of soluble ferric salt, trisodium citrate and an ethanol/water mixture, mixing, and carrying out hydrothermal reaction for 4 hours at 200 ℃; wherein the volume ratio of ethanol to water is 85;
2) dispersing the product obtained in the step 1 in an alcohol solvent, adding water and tetraethyl silicate, and stirring for 5 hours at 40 ℃; filtering and washing; wherein the molar ratio of iron to silicon is 2;
3) sequentially adding the product in the step 2 into hexadecyltrimethylamine bromide, water, a phenol compound, absolute ethyl alcohol, ammonia water and an aldehyde compound, and stirring for 5 hours at 50 ℃; filtering and washing;
4) adding the product of the step 3 into N2Carbonizing at 600 ℃ for 5 hours in the atmosphere;
5) repeating the cycle of the steps 1,2,3 and 4 for 2 times by using the product obtained in the step 4;
6) putting the product obtained in the step 5) into a strong alkali solution for 10 hours; washing and drying;
7) mixing the product obtained in the step 6 with iodine, and performing solid solution at 150 ℃ for 5 hours; then solid dissolving for 5 hours at 500 ℃; obtaining the iron-based-carbon composite material with a three-layer core-shell structure.
The component design of the iron-based-carbon composite material with the three-layer core-shell structure comprises the following steps:
5) a first layer: 0.06mol of ferric acetate; 0.03mol tetraethyl silicate; 0.15mol of phloroglucinol; 0.15mol of acetaldehyde; 0.06mol of iodine;
a second layer: 0.06mol of ferric acetate; 0.03mol tetraethyl silicate; 0.2mol of phloroglucinol; 0.2mol of acetaldehyde; 0.06mol of iodine;
and a third layer: 0.06mol of ferric acetate; 0.03mol tetraethyl silicate; 0.25mol of phloroglucinol; 0.25mol of acetaldehyde; 0.06mol of iodine;
6) a first layer: 0.1mol of ferric acetate; 0.04mol of tetraethyl silicate; 0.2mol of p-phenol; 0.16mol of butyraldehyde; 0.1mol of iodine;
a second layer: 0.1mol of ferric acetate; 0.04mol of tetraethyl silicate; 0.25mol of p-phenol; 0.22mol of butyraldehyde; 0.1mol of iodine;
and a third layer: 0.1mol of ferric acetate; 0.04mol of tetraethyl silicate; 0.3mol of p-phenol; 0.28mol of butyraldehyde; 0.1mol of iodine;
microstructure display: the iron-based-carbon composite material has a micro-nano core-shell structure, and the carbon core shell covers the iron-based electrode material; the electrochemical test results show that: the iron-based-carbon composite material has good electrochemical performance.
The above-described embodiments of the patent are intended to be illustrative, but not limiting, of the scope of the patent, which is included for the purpose of better understanding the patent by those skilled in the art; any equivalent alterations or modifications made according to the spirit of the disclosure of this patent are intended to be included in the scope of this patent.

Claims (5)

1. The invention relates to a preparation method of an iron-based-carbon composite material with a core-shell structure, which is characterized by comprising the following steps: taking soluble ferric salt as a raw material, performing ferric salt hydrothermal reaction, tetraethyl silicate hydrolysis and polymer coating, repeatedly circulating for 0-3 times, performing strong alkali treatment, carbonizing, and finally reacting with iodine to obtain the iron-based-carbon composite material with the core-shell structure; the soluble ferric salt is one of ferric chloride, ferric bromide, ferric nitrate and ferric acetate; the polymer precursor is phenol compound and aldehyde compound; the phenol compound is one of phenol, m-diphenol, m-triphenol, p-phenol and o-phenol; the aldehyde compound is one of formaldehyde, acetaldehyde, propionaldehyde and butyraldehyde; a preparation method of an iron-based-carbon composite material with a core-shell structure comprises the following steps:
1) weighing a certain mass of soluble ferric salt, trisodium citrate and an ethanol/water mixture, mixing, and carrying out hydrothermal reaction at 100-240 ℃ for 3-20 hours; wherein the volume ratio of ethanol to water is 80-100;
2) dispersing the product obtained in the step 1 in an alcohol solvent, adding water and tetraethyl silicate, and stirring for 5-10 hours at the temperature of 20-70 ℃; filtering and washing; wherein the molar ratio of iron to silicon is 2-5;
3) sequentially adding the product in the step 2 into hexadecyltrimethylamine bromide, water, a phenol compound, absolute ethyl alcohol, ammonia water and an aldehyde compound, and stirring for 5-10 hours at the temperature of 20-70 ℃; filtering and washing;
4) adding the product of the step 3 into N2Carbonizing at the temperature of 800 ℃ for 2-10h under the atmosphere of 400-;
5) repeating the product of the step 4 for 0-3 times of cycles of the step 1, the step 2, the step 3 and the step 4;
6) putting the product obtained in the step 5 into a strong alkali solution for 5-10 hours; washing and drying;
7) mixing the product obtained in the step 6 with iodine, and carrying out solid solution at the temperature of 100-200 ℃ for 2-10 hours; then solid solution is carried out for 1-5 hours at the temperature of 400-800 ℃; obtaining the iron-based-carbon composite material with the core-shell structure; wherein the molar ratio of iodine to iron is 0.2-1.2.
2. The preparation method of the iron-based carbon composite material with the core-shell structure, according to claim 1, is characterized in that: the iron-based-carbon composite material contains 1-4 layers of core-shell structures.
3. The preparation method of the iron-based carbon composite material with the core-shell structure, according to claim 1, is characterized in that: the iron-based-carbon composite contains micro-nano structures.
4. The preparation method of the iron-based carbon composite material with the core-shell structure, according to claim 1, is characterized in that: the molar ratio of the iron element to the phenol compound is 0.5-5.
5. The preparation method of the iron-based carbon composite material with the core-shell structure, according to claim 1, is characterized in that: the molar ratio of the phenol compound to the aldehyde compound is 1-1.5.
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