CN112234204A - Carbon cloth loaded SiO2Coated Sb2O5Composite self-supporting electrode material and preparation method thereof - Google Patents

Carbon cloth loaded SiO2Coated Sb2O5Composite self-supporting electrode material and preparation method thereof Download PDF

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CN112234204A
CN112234204A CN202011106686.4A CN202011106686A CN112234204A CN 112234204 A CN112234204 A CN 112234204A CN 202011106686 A CN202011106686 A CN 202011106686A CN 112234204 A CN112234204 A CN 112234204A
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carbon cloth
electrode material
coated
sio
supporting electrode
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费杰
王娜
黄剑锋
曹丽云
许占位
李嘉胤
郑欣慧
李盟
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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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
    • H01M4/62—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
    • 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • 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 discloses a carbon cloth loaded SiO2Coated Sb2O5The invention discloses a composite self-supporting electrode material and a preparation method thereof, wherein the preparation method comprises the following specific steps: 1): adding antimony trichloride and sodium hydroxide into deionized water to form a reaction precursor solution A; 2): adding a silicon dioxide solution into the reaction precursor solution A, and soaking the carbon cloth subjected to anodic oxidation activation in the reaction precursor; 3): transferring the carbon cloth obtained in the step 2) and the reaction precursor liquid into a reactor, carrying out hydrothermal reaction at the temperature of 150-180 ℃, cooling to room temperature after the reaction is finished, taking out the carbon cloth, cleaning and drying to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material. The preparation method disclosed by the invention has the advantages of simplicity, short preparation period, high repeatability, good electrochemical performance of the prepared product, low cost, environmental friendliness, controllable structural design and the like.

Description

Carbon cloth loaded SiO2Coated Sb2O5Composite self-supporting electrode material and preparation method thereof
Technical Field
The invention relates to a new energy material technology, in particular to a carbon cloth loaded SiO2Coated Sb2O5A composite self-supporting electrode material and a preparation method thereof.
Background
Compared with the traditional electrode preparation, the self-supporting electrode has the advantages that the addition of a conductive agent and a binder is reduced, the proportion of active substances is increased, the contact resistance between an electrolyte and an active site is reduced, the use of a copper foil or an aluminum foil as a current collector is avoided, and the cost is reduced. Carbon cloth is one type of cloth that has both the porosity and flexibility of a fabric and the electrical conductivity of a carbon material. As a self-supporting electrode of a lithium/sodium ion battery, the self-supporting electrode not only can load active substances, but also is beneficial to the diffusion of electrolyte and the shuttling of lithium and sodium ions, and is an ideal flexible self-supporting substrate material of the battery. At present, the reports related to the carbon cloth loaded with active substances as the negative electrode material of the sodium ion battery not only directly load single-component active substances: such as Sb2O3、TiO2、FeP、MoS2、MoO3、Ni3V2O8And the like, also present are active species supported and modified such as C/SnO2、FeS/C、TiO2/SnS2and/N-C and the like. E.g. Hou X et al in SnO2Synthesizing C/SnO on/CC by solvothermal method and atomic deposition method (ALD) respectively2C and Al2O3/SnO2Two kinds of composite materials,/CC, C/SnO2The specific capacity of the/CC serving as the negative electrode material of the sodium ion battery reaches under the current density of 134 mA.g < -1 >To 501 mAh.g-1; al (Al)2O3/SnO2The specific capacity of the/CC used as the cathode material of the sodium ion battery reaches 375 mAh.g-1 SnO2 Coated Carbon Cloth with Surface Modification as Na-ion Battery Anode[J].Nano Energy,2015,16:399-407.]. The Xiang Wei et al combines hydrothermal method with carbonization method to prepare C/FeS/CC Sodium ion battery Flexible self-supporting Electrode material, and the specific capacity is kept at 365mAh g-1[ FeS @ C on Carbon Cloth as Flexible Electrode for bed Lithium and Sodium Storage [ J ] after circulating 100 circles under the condition of current density of 0.15C (91.35mA g-1)].ACS Applied Materials&Interfaces,2015,7(5 0):27804-27809.]。
Therefore, the electrochemical performance of a single metal compound as an active material can be improved by the compounding method, however, a carbon material is often adopted in the compounding process, the inherent specific capacity of the carbon material is low, and the capability of improving the specific capacity property of the composite material is limited, so that a new material capable of being used for compounding needs to be developed. Researches find that the morphology of the compound has great influence on the performance of the sodium-ion battery, and at present, SiO with special morphology can be controllably synthesized on carbon cloth2Coated Sb2O5No report exists on the use of the composite as a battery self-supporting material, so that SiO with a special morphology can be controllably synthesized on carbon cloth2Coated Sb2O5The composite has important significance for improving the specific capacity property of the composite material.
Disclosure of Invention
The invention aims to provide a carbon cloth loaded SiO2Coated Sb2O5Composite self-supporting electrode materials, and methods of making the same. The preparation method has simple process, can control the appearance of the prepared product, and loads the prepared carbon cloth with SiO2Coated Sb2O5The composite self-supporting electrode material can show good electrochemical performance when applied to a negative electrode of a sodium-ion battery.
The purpose of the invention is realized by the following technical scheme:
carbon cloth loaded SiO2Coating ofSb2O5The preparation method of the composite self-supporting electrode material comprises the following specific steps:
step (1): adding 0.57-0.9 g of antimony trichloride and 0.3-0.5 g of sodium hydroxide into 20-30 mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 0.25-1 mL of silicon dioxide solution into the reaction precursor solution A to obtain a solution B, and soaking the carbon cloth subjected to anodic oxidation activation into the solution B;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reaction container, carrying out hydrothermal reaction for 12-48 h at the temperature of 150-180 ℃, cooling to room temperature after the reaction is finished, taking out the carbon cloth, cleaning and drying to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
Further, the mass concentration of the silicon dioxide solution in the step (2) is 30%, and the pH value is 9.1.
Further, the electrolyte used in the anodic oxidation activation in the step (2) is 20-25 g/L ammonium dihydrogen phosphate, the anodic oxidation voltage is 5V, and the anodic oxidation time is 3-5 min.
Further, the dipping time of the carbon cloth in the step (2) is 10-60 min.
Further, the reaction vessel in the step (3) is a homogeneous reactor, and the rotation speed of the homogeneous reactor is 10 r/min.
The carbon cloth loaded SiO prepared by the preparation method2Coated Sb2O5A composite self-supporting electrode material.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method prepares SiO on the carbon cloth by a simple one-step hydrothermal method2Coated Sb2O5The prepared product of the composite material has uniform appearance, the preparation method is simple, the preparation period is short, the repeatability is strong, the specific capacity of the composite material is improved, and the composite material has important significance for preparing the composite carbon cloth flexible self-supporting electrode material.
According to the inventionCarbon cloth loaded SiO obtained by preparation method2Coated Sb2O5A composite self-supporting electrode material is based on carbon cloth as a substrate, the carbon cloth provides a stable electron transmission path with a supporting structure for an active material, and Sb2O5Has high theoretical specific energy storage capacity, and more importantly, SiO2The nano particles are uniformly coated on the Sb2O5The particle surface plays a role of physical confinement, and the confinement can effectively inhibit Sb2O5Volume expansion and contraction during charge and discharge, thereby preventing Sb2O5The energy is dropped off, and the energy storage stability is improved; the unique shape of the composite material is beneficial to the infiltration and the preservation of the electrolyte, the rapid transmission of electrons is accelerated, and the performances of sodium storage and the like of the composite material are improved. Therefore, the carbon cloth obtained by the preparation method of the invention is loaded with SiO2Coated Sb2O5When the composite self-supporting electrode material is applied to the cathode of a lithium/sodium ion battery, the composite self-supporting electrode material can show good electrochemical performance, and has the advantages of low cost, environmental friendliness, controllable structural design, good safety and the like.
Drawings
FIG. 1 shows a SiO supported carbon cloth prepared in example 1 of the present invention2Coated Sb2O5An X-ray diffraction pattern of the composite self-supporting electrode material;
FIG. 2 shows a SiO supported carbon cloth prepared in example 1 of the present invention2Coated Sb2O5Scanning electron micrographs (low magnification) of the composite self-supporting electrode material;
FIG. 3 shows SiO supported carbon cloth prepared in example 1 of the present invention2Coated Sb2O5Scanning electron micrographs (low magnification) of the composite self-supporting electrode material;
FIG. 4 shows SiO supported carbon cloth prepared in example 1 of the present invention2Coated Sb2O5Scanning electron micrographs (high magnification) of the composite self-supporting electrode material;
FIG. 5 shows SiO supported carbon cloth prepared in example 1 of the present invention2Coated Sb2O5A transmission electron microscope photograph of the composite self-supporting electrode material;
FIG. 6 shows SiO supported carbon cloth prepared in example 1 of the present invention2Coated Sb2O5An electrochemical cycle performance diagram of the composite self-supporting lithium ion battery electrode material;
FIG. 7 shows SiO supported carbon cloth prepared in example 1 of the present invention2Coated Sb2O5Electrochemical cycling performance diagram of the composite self-supporting sodium ion battery electrode material.
Detailed Description
The invention is described in further detail below with reference to the figures and specific embodiments.
Example 1
The carbon cloth of the invention loads SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material comprises the following specific steps:
step (1): adding 0.57g of antimony trichloride and 0.3g of sodium hydroxide into 20mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 0.25mL of silicon dioxide solution with the mass concentration of 30% and the pH value of 9.1 into the reaction precursor solution A to obtain a solution B, carrying out anodic oxidation activation treatment on the carbon cloth by using 20-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, the anodic oxidation time is 3-5 min, and soaking the carbon cloth subjected to anodic oxidation activation in the solution B for 10 min;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reactor, wherein the reactor is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is set to be 10r/min, carrying out hydrothermal reaction for 48h at 180 ℃, cooling the reaction product to room temperature along with the homogeneous reactor after the reaction is finished, taking out the carbon cloth, repeatedly cleaning the carbon cloth with deionized water, and drying the carbon cloth to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
SiO is loaded on the carbon cloth prepared in the embodiment2Coated Sb2O5Performing characterization test on the composite self-supporting electrode material:
analysis of the carbon cloth-supported SiO with the Nippon Denshi D/max2000 PCX-ray diffractometer2Coated Sb2O5The result of compounding the self-supporting electrode material is shown in FIG. 1, and it can be seen from FIG. 1 that the composite material is mixed with Sb with PDF number of 11-06902O5SiO with structure and PDF number of 76-09332Consistently, successful preparation of SiO on carbon cloth substrates was demonstrated2Coated Sb2O5A composite material.
The SiO supported carbon cloth prepared in this example was observed with a field emission scanning electron microscope (FEI S-4800, USA)2Coated Sb2O5The results of the composite self-supporting electrode material at low magnification are shown in FIGS. 2 and 3, from which it can be seen that SiO2The nano particles are uniformly coated on the Sb2O5The periphery is neat and beautiful in appearance; the results at high magnification are shown in FIG. 4, from which it can be further found that Sb is a very important factor2O5The outer surface is coated with SiO2Surrounded by particles.
Further, the SiO supported carbon cloth prepared in this example was observed with a transmission electron microscope of model G2F 20, FEI Co2Coated Sb2O5Composite self-supporting electrode material, SiO, as can be seen in FIG. 52The nanoparticles are coated on Sb2O5And (4) periphery.
The carbon cloth prepared by the embodiment is loaded with SiO2Coated Sb2O5When the composite self-supporting electrode material is used as a lithium/sodium ion battery cathode material, a CR2032 type battery is assembled, and the electrochemical performance test is carried out by using a blue test system CT2001 system, and the results are shown in FIGS. 6 and 7, and the battery shows good rate capability, higher electrochemical capacity and stability.
Example 2
The carbon cloth of the invention loads SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material comprises the following specific steps:
step (1): adding 0.57g of antimony trichloride and 0.3g of sodium hydroxide into 20mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 1mL of silicon dioxide solution with the mass concentration of 30% and the pH value of 9.1 into the reaction precursor solution A to obtain a solution B, carrying out anodic oxidation activation treatment on the carbon cloth by using 20-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, the anodic oxidation time is 3-5 min, and soaking the carbon cloth subjected to anodic oxidation activation in the solution B for 10 min;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reactor, wherein the reactor is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is set to be 10r/min, carrying out hydrothermal reaction for 24 hours at 180 ℃, cooling the reaction product to room temperature along with the homogeneous reactor after the reaction is finished, taking out the carbon cloth, repeatedly cleaning the carbon cloth with deionized water, and drying the carbon cloth to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
Example 3
The carbon cloth of the invention loads SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material comprises the following specific steps:
step (1): adding 0.74g of antimony trichloride and 0.35g of sodium hydroxide into 20mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 0.75mL of silicon dioxide solution with the mass concentration of 30% and the pH value of 9.1 into the reaction precursor solution A to obtain a solution B, carrying out anodic oxidation activation treatment on the carbon cloth by using 20-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, the anodic oxidation time is 3-5 min, and soaking the carbon cloth subjected to anodic oxidation activation in the solution B for 30 min;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reactor, wherein the reactor is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is set to be 10r/min, carrying out hydrothermal reaction for 48h at 150 ℃, cooling the reaction product to room temperature along with the homogeneous reactor after the reaction is finished, taking out the carbon cloth, repeatedly cleaning the carbon cloth with deionized water, and drying the carbon cloth to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
Example 4
The carbon cloth of the invention loads SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material comprises the specific stepsComprises the following steps:
step (1): adding 0.8g of antimony trichloride and 0.4g of sodium hydroxide into 30mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 0.5mL of silicon dioxide solution with the mass concentration of 30% and the pH value of 9.1 into the reaction precursor solution A to obtain a solution B, carrying out anodic oxidation activation treatment on the carbon cloth by using 20-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, the anodic oxidation time is 3-5 min, and soaking the carbon cloth subjected to anodic oxidation activation in the solution B for 20 min;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reactor, wherein the reactor is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is set to be 10r/min, carrying out hydrothermal reaction for 24 hours at the temperature of 150 ℃, cooling the reaction product to room temperature along with the homogeneous reactor after the reaction is finished, taking out the carbon cloth, repeatedly cleaning the carbon cloth with deionized water, and drying the carbon cloth to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
Example 5
The carbon cloth of the invention loads SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material comprises the following specific steps:
step (1): adding 0.57g of antimony trichloride and 0.3g of sodium hydroxide into 30mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 0.25mL of silicon dioxide solution with the mass concentration of 30% and the pH value of 9.1 into the reaction precursor solution A to obtain a solution B, carrying out anodic oxidation activation treatment on the carbon cloth by using 20-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, the anodic oxidation time is 3-5 min, and soaking the carbon cloth subjected to anodic oxidation activation in the solution B for 10 min;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reactor, wherein the reactor is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is set to be 10r/min, carrying out hydrothermal reaction for 48h at 180 ℃, cooling the reaction product to room temperature along with the homogeneous reactor after the reaction is finished, taking out the carbon cloth, repeatedly cleaning the carbon cloth with deionized water, and drying the carbon cloth to obtain the carbon cloth negativeSiO-Supported SiO 22Coated Sb2O5A composite self-supporting electrode material.
Example 6
The carbon cloth of the invention loads SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material comprises the following specific steps:
step (1): adding 0.57g of antimony trichloride and 0.3g of sodium hydroxide into 20mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 1mL of silicon dioxide solution with the mass concentration of 30% and the pH value of 9.1 into the reaction precursor solution A to obtain a solution B, carrying out anodic oxidation activation treatment on the carbon cloth by using 20-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, the anodic oxidation time is 3-5 min, and soaking the carbon cloth subjected to anodic oxidation activation into the solution B for 20 min;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reactor, wherein the reactor is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is set to be 10r/min, carrying out hydrothermal reaction for 24 hours at 180 ℃, cooling the reaction product to room temperature along with the homogeneous reactor after the reaction is finished, taking out the carbon cloth, repeatedly cleaning the carbon cloth with deionized water, and drying the carbon cloth to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
Example 7
The carbon cloth of the invention loads SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material comprises the following specific steps:
step (1): adding 0.68g of antimony trichloride and 0.34g of sodium hydroxide into 20mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 0.6mL of silicon dioxide solution with the mass concentration of 30% and the pH value of 9.1 into the reaction precursor solution A to obtain a solution B, carrying out anodic oxidation activation treatment on the carbon cloth by using 20-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, the anodic oxidation time is 3-5 min, and soaking the carbon cloth subjected to anodic oxidation activation in the solution B for 30 min;
and (3): dissolving in the step (2)Transferring the liquid B and the impregnated carbon cloth into a reactor, preferably a homogeneous reactor, setting the rotation speed of the homogeneous reactor at 10r/min, carrying out hydrothermal reaction for 48h at 180 ℃, cooling the reaction product to room temperature along with the homogeneous reactor after the reaction is finished, taking out the carbon cloth, repeatedly cleaning the carbon cloth by deionized water, and drying the carbon cloth to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
Example 8
The carbon cloth of the invention loads SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material comprises the following specific steps:
step (1): adding 0.77g of antimony trichloride and 0.4g of sodium hydroxide into 30mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 0.8mL of silicon dioxide solution with the mass concentration of 30% and the pH value of 9.1 into the reaction precursor solution A to obtain a solution B, carrying out anodic oxidation activation treatment on the carbon cloth by using 20-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, the anodic oxidation time is 3-5 min, and soaking the carbon cloth subjected to anodic oxidation activation in the solution B for 30 min;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reactor, wherein the reactor is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is set to be 10r/min, carrying out hydrothermal reaction for 48h at 180 ℃, cooling the reaction product to room temperature along with the homogeneous reactor after the reaction is finished, taking out the carbon cloth, repeatedly cleaning the carbon cloth with deionized water, and drying the carbon cloth to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
Example 9
The carbon cloth of the invention loads SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material comprises the following specific steps:
step (1): adding 0.9g of antimony trichloride and 0.3g of sodium hydroxide into 20mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 0.25mL of silicon dioxide solution with the mass concentration of 30% and the pH value of 9.1 into the reaction precursor solution A to obtain a solution B, carrying out anodic oxidation activation treatment on the carbon cloth by using 20-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, the anodic oxidation time is 3-5 min, and soaking the carbon cloth subjected to anodic oxidation activation in the solution B for 30 min;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reactor, wherein the reactor is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is set to be 10r/min, carrying out hydrothermal reaction for 12h at 180 ℃, cooling the reaction product to room temperature along with the homogeneous reactor after the reaction is finished, taking out the carbon cloth, repeatedly cleaning the carbon cloth with deionized water, and drying the carbon cloth to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
Example 10
The carbon cloth of the invention loads SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material comprises the following specific steps:
step (1): adding 0.57g of antimony trichloride and 0.5g of sodium hydroxide into 30mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 1mL of silicon dioxide solution with the mass concentration of 30% and the pH value of 9.1 into the reaction precursor solution A to obtain a solution B, carrying out anodic oxidation activation treatment on the carbon cloth by using 20-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, the anodic oxidation time is 3-5 min, and soaking the carbon cloth subjected to anodic oxidation activation in the solution B for 30 min;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reactor, wherein the reactor is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is set to be 10r/min, carrying out hydrothermal reaction for 12h at 150 ℃, cooling the reaction product to room temperature along with the homogeneous reactor after the reaction is finished, taking out the carbon cloth, repeatedly cleaning the carbon cloth with deionized water, and drying the carbon cloth to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
In conclusion, the hydrothermal method provided by the invention for preparing carbon cloth loaded SiO2Coated Sb2O5The method for compounding the self-supporting electrode material can be used for preparing carbon by a simple one-step hydrothermal methodPreparing SiO on cloth2Coated Sb2O5The prepared product of the composite material has uniform appearance, simple preparation method, short preparation period and strong repeatability, and has important significance for preparing the composite carbon cloth flexible self-supporting electrode material. More importantly, flower-like SiO2Uniformly coated on Sb2O5The periphery plays a role of physical confinement, and the confinement can effectively inhibit Sb2O5Volume expansion and contraction during charge and discharge, and protection of polyhedron Sb2O5And in addition, the unique shape of the composite material is beneficial to the infiltration and the storage of the electrolyte, the rapid transmission of electrons is accelerated, and the sodium storage performance of the composite material is improved. The preparation method is simple, short in preparation period and high in repeatability, and has important significance for preparing the composite carbon cloth flexible self-supporting electrode material.

Claims (6)

1. Carbon cloth loaded SiO2Coated Sb2O5The preparation method of the composite self-supporting electrode material is characterized by comprising the following specific steps of:
step (1): adding 0.57-0.9 g of antimony trichloride and 0.3-0.5 g of sodium hydroxide into 20-30 mL of deionized water to obtain a reaction precursor solution A;
step (2): adding 0.25-1 mL of silicon dioxide solution into the reaction precursor solution A to obtain a solution B, and soaking the carbon cloth subjected to anodic oxidation activation into the solution B;
and (3): transferring the solution B in the step (2) and the impregnated carbon cloth into a reaction container, carrying out hydrothermal reaction for 12-48 h at the temperature of 150-180 ℃, cooling to room temperature after the reaction is finished, taking out the carbon cloth, cleaning and drying to obtain the carbon cloth loaded with SiO2Coated Sb2O5A composite self-supporting electrode material.
2. The carbon cloth-supported SiO of claim 12Coated Sb2O5The preparation method of the composite self-supporting electrode material is characterized by comprising the following steps: the mass concentration of the silicon dioxide solution in the step (2) is 30%, and the pH value is 9.1.
3. The carbon cloth-supported SiO of claim 12Coated Sb2O5The preparation method of the composite self-supporting electrode material is characterized by comprising the following steps: in the step (2), 20-25 g/L of ammonium dihydrogen phosphate is used as an electrolyte for anodic oxidation activation, the anodic oxidation voltage is 5V, and the anodic oxidation time is 3-5 min.
4. The carbon cloth-supported SiO of claim 12Coated Sb2O5The preparation method of the composite self-supporting electrode material is characterized by comprising the following steps: and (3) dipping the carbon cloth in the step (2) for 10-60 min.
5. The carbon cloth-supported SiO of claim 12Coated Sb2O5The preparation method of the composite self-supporting electrode material is characterized by comprising the following steps: the reaction vessel in the step (3) is a homogeneous reactor, and the rotating speed of the homogeneous reactor is 10 r/min.
6. Carbon cloth loaded SiO prepared by the method of any one of the preceding claims2Coated Sb2O5A composite self-supporting electrode material.
CN202011106686.4A 2020-10-16 2020-10-16 Carbon cloth loaded SiO2Coated Sb2O5Composite self-supporting electrode material and preparation method thereof Pending CN112234204A (en)

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