CN112038623A - Sb based on controllable construction of carbon cloth substrate2O4Self-supporting electrode material for sodium ion battery cathode and preparation method thereof - Google Patents

Sb based on controllable construction of carbon cloth substrate2O4Self-supporting electrode material for sodium ion battery cathode and preparation method thereof Download PDF

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CN112038623A
CN112038623A CN202010939853.7A CN202010939853A CN112038623A CN 112038623 A CN112038623 A CN 112038623A CN 202010939853 A CN202010939853 A CN 202010939853A CN 112038623 A CN112038623 A CN 112038623A
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carbon cloth
ion battery
self
electrode material
preparation
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费杰
王娜
黄剑锋
曹丽云
许占位
李嘉胤
郑欣慧
杨甜
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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
    • H01M4/36—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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01M4/62—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
    • 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 controllable Sb structure based on a carbon cloth substrate2O4A self-supporting electrode material for a sodium ion battery cathode and a preparation method thereof. The preparation method comprises the following specific steps: 1): dissolving antimony trichloride in a solvent to obtain an antimony solution, wherein the solvent is one or two of absolute ethyl alcohol and deionized water, adjusting the pH of the antimony solution to 2-7 without adjusting or by using NaOH, and soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution; 2): transferring the carbon cloth and the antimony solution obtained in the step 1)Carrying out solvent thermal or hydrothermal reaction in a reaction container, cooling after the reaction is finished, taking out the carbon cloth, washing and drying to obtain Sb controllably constructed based on the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery. The preparation method provided by the invention is simple in process, good in controllability and short in preparation period, is suitable for large-scale industrial production, and the obtained self-supporting electrode material is uniform in shape and shows good electrochemical performance when being used as a self-supporting cathode material of a sodium ion battery.

Description

Sb based on controllable construction of carbon cloth substrate2O4Self-supporting electrode material for sodium ion battery cathode and preparation method thereof
Technical Field
The invention relates to the field of new energy materials, in particular to a method for controllably constructing Sb based on a carbon cloth substrate2O4A self-supporting electrode material for a sodium ion battery cathode and a preparation method thereof.
Background
With the advent of crimpable, foldable, wearable, and implantable electronic devices, research into flexible electrode materials has also been spotlighted. The carbon cloth has high mechanical strength and large specific surface area, and is beneficial to attaching active substances, so that the addition of an insulating binder can be avoided; in addition, the porous space structure of the carbon cloth is beneficial to electrolyte diffusion and ion and electron transfer, and becomes the first choice of the self-supporting electrode substrate material of the lithium/sodium ion battery. In order to improve the specific capacity performance of the carbon cloth-based electrode material, a metal simple substance, a metal compound and a composite material are often used as active materials to be loaded on the carbon cloth substrate.
Sb2O4The theoretical capacity of the anode is up to 1227mAhg-1It is an NIBs anode material with wide application prospect. However, in practical application, the antimony oxide anode material usually has the problems of large voltage lag, low reversibility and the like, so researchers often modify the antimony oxide anode material, and the antimony oxide anode material is compounded with a carbon material by a common method such as Kiruthiga RamakrishhnanEtc. to prepare Sb2O4Particulate @ rGO composites at a current density of 0.6Ag-1The capacity can be kept to 626mAhg after 500 cycles-1. Also for example Sb prepared by Gui-Zhi Wang et al2O4nanorod/RGO composite material with current density of 0.05Ag-1The capacity can be maintained to be 551 +/-5 mAhg after 100 cycles-1。
The structure determines the performance, the growth appearance of the active substance on the carbon cloth plays an important role in playing the electrochemical performance, and Sb with different appearances can be controllably constructed on the carbon cloth2O4There is no report yet. Therefore, Sb with special appearance can be controllably synthesized on the carbon cloth2O4Therefore, a new technical means can be provided for improving the electrochemical performance of the battery.
Disclosure of Invention
The invention aims to provide a method for controllably constructing Sb based on a carbon cloth substrate2O4A self-supporting electrode material for a sodium ion battery cathode and a preparation method thereof. The preparation method provided by the invention is simple in process, good in controllability and short in preparation period, and is suitable for large-scale industrial production.
The purpose of the invention is realized by the following technical scheme:
sb based on controllable construction of carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery comprises the following specific steps:
step (1): dissolving 0.5-0.8 g of antimony trichloride in a solvent of less than or equal to 40mL to obtain an antimony solution, wherein the solvent is one or a mixed solution of absolute ethyl alcohol and deionized water, and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution, or regulating the pH value of the antimony solution to 2-7 by using a sodium hydroxide aqueous solution and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution obtained in the step (1) into a reaction container, and feeding at the temperature of 150-180 DEG CPerforming solvothermal or hydrothermal reaction for 12-48 h, cooling to room temperature after the reaction is finished, taking out the carbon cloth, washing and drying to obtain Sb controllably constructed based on the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
Further, in the step (1), 0.6g/mL of aqueous sodium hydroxide solution is used to adjust the pH of the antimony solution.
Further, the electrolyte used in the anodic oxidation treatment in the step (1) is 10-25 g/L ammonium dihydrogen phosphate, the anodic oxidation voltage is 5V, and the time is 3-7 min.
Further, the reaction vessel in the step (2) is a homogeneous reactor, and the rotation speed of the homogeneous reactor is 10 r/min.
Sb prepared by any of the preparation methods and based on carbon cloth substrate controllable construction2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
Compared with the prior art, the invention has the following beneficial effects:
the invention takes absolute ethyl alcohol or deionized water or the mixed solution of the absolute ethyl alcohol and the deionized water as a solvent, and SbCl3As an antimony source, pure-phase Sb is prepared by adopting a one-step solvothermal method or hydrothermal method2O4Crystals, Sb prepared on carbon cloth when the solvent is pure absolute ethanol2O4The shape is uniform rice grain shape, when the solvent is pure deionized water, the flower shape is self-assembled by nanorods with two tips, the size is larger, and when the solvent is a mixed solution of absolute ethyl alcohol and deionized water, Sb synthesized on carbon cloth2O4The flower is also in a flower shape, the size of the flower is smaller and regular than that of the flower prepared by pure water solvent, and the integral uniformity of the flower is better than that of the flower prepared by pure water solvent. The preparation method has the advantages of simple process, good controllability and short preparation period, and is suitable for large-scale industrial production.
The self-supporting electrode material prepared by the preparation method has uniform appearance, and Sb prepared on the carbon cloth2O4Has special appearance and high theoretical specific capacity, so the lithium iron phosphate shows good electrochemistry when being used as a self-supporting cathode material of a sodium ion batteryAnd (4) performance.
Drawings
FIG. 1 shows a controllable construction of Sb based on a carbon cloth substrate prepared in example 1 of the present invention2O4X-ray diffraction pattern of self-supporting electrode material for sodium ion battery cathode;
FIG. 2 shows a controllable Sb structure based on a carbon cloth substrate prepared in example 1 of the present invention2O4Scanning electron microscope photos of the self-supporting electrode material for the cathode of the sodium ion battery;
FIG. 3 shows a controllable Sb structure based on a carbon cloth substrate prepared in example 2 of the present invention2O4Scanning electron microscope photos of the self-supporting electrode material for the cathode of the sodium ion battery;
FIG. 4 shows a controllable Sb structure based on a carbon cloth substrate prepared in example 2 of the present invention2O4A graph of electrochemical cycling performance of a self-supporting electrode material for a sodium ion battery negative electrode;
FIG. 5 shows a controllable Sb structure based on a carbon cloth substrate prepared in example 3 of the present invention2O4Scanning electron microscope photographs of self-supporting electrode materials for the negative electrode of the sodium ion battery.
Detailed Description
The invention is described in further detail below with reference to the figures and specific embodiments.
Example 1
The invention discloses a method for controllably constructing Sb based on a carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery comprises the following specific steps:
step (1): dissolving 0.57g of antimony trichloride in 20mL of absolute ethyl alcohol pure solvent to obtain an antimony solution, carrying out anodic oxidation treatment on the carbon cloth by using 10-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, and the time is 3-7 min, and soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution in the step (1) into a reaction vessel, wherein the reaction vessel is preferably a homogeneous reactor, the rotating speed of the homogeneous reactor is 10r/min, carrying out solvothermal or hydrothermal reaction for 48h at 180 ℃ in the homogeneous reactor, and finishing the reactionThen cooling to room temperature, taking out the carbon cloth, washing and drying to obtain Sb controllably constructed based on the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
Analysis of Sb controllably constructed on the basis of a carbon cloth substrate prepared in this example by means of a Japanese science D/max2000 PCX-ray diffractometer2O4Self-supporting electrode material for sodium ion battery negative electrode, namely Sb2O4Carbon cloth samples, as shown in FIG. 1, Sb2O4(ii) Sb of 78-2006 in PDF number and/or carbon cloth sample2O4The structures are consistent, which indicates that Sb is successfully synthesized2O4A carbon cloth. The sample was observed with a NULL type scanning electron microscope (FEI, USA), and the result is shown in FIG. 2, which shows that Sb is produced2O4Uniformly grown on carbon cloth, Sb2O4Is shaped like rice grains with two sharp ends.
Example 2
The invention discloses a method for controllably constructing Sb based on a carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery comprises the following specific steps:
step (1): dissolving 0.57g of antimony trichloride in a mixed solvent of 10mL of anhydrous ethanol and 10mL of deionized water to obtain an antimony solution, adjusting the pH value of the antimony solution to 3 by using 0.6g/mL of sodium hydroxide aqueous solution, carrying out anodic oxidation treatment on carbon cloth by using 10-25 g/L of ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, and the time is 3-7 min, and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution in the step (1) into a reaction vessel, wherein the reaction vessel is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is 10r/min, carrying out solvothermal or hydrothermal reaction for 48h at 180 ℃ in the homogeneous reactor, cooling to room temperature after the reaction is finished, taking out the carbon cloth, washing and drying to obtain the Sb controllably constructed based on the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
The carbon-based cloth substrate prepared in this example was observed with a scanning electron microscope of model S-4800, FEI, USAControllable construction of Sb2O4The self-supporting electrode material for the negative electrode of the sodium ion battery was obtained, and as a result, it can be seen from FIG. 3 that Sb was produced2O4Uniformly grown on carbon cloth, Sb2O4Self-assembling the nano-rods into flower shapes. Sb controllable construction based on prepared carbon cloth substrate2O4The self-supporting electrode material for the sodium ion battery cathode is a sodium ion battery cathode material, a CR2032 type battery is assembled, electrochemical performance test is carried out by a Wuhan blue electric test system CT2100, the result is shown in figure 4, and it can be seen from the figure that when the current density returns to 500mAg after the multiplying power performance test-1The specific discharge capacity of the battery is 600mAhg-1And high electrochemical performance is shown.
Example 3
The invention discloses a method for controllably constructing Sb based on a carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery comprises the following specific steps:
step (1): dissolving 0.57g of antimony trichloride in 20mL of deionized water to obtain an antimony solution, adjusting the pH value of the antimony solution to 2 by using a 0.6g/mL sodium hydroxide aqueous solution, carrying out anodic oxidation treatment on a carbon cloth by using 10-25 g/L ammonium dihydrogen phosphate as an electrolyte, wherein the anodic oxidation voltage is 5V, and the time is 3-7 min, and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution in the step (1) into a reaction vessel, wherein the reaction vessel is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is 10r/min, carrying out solvothermal or hydrothermal reaction for 48h at 180 ℃ in the homogeneous reactor, cooling to room temperature after the reaction is finished, taking out the carbon cloth, washing and drying to obtain the Sb controllably constructed based on the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
Sb prepared in the present example and based on the controlled construction of a carbon cloth substrate was observed by a NULL-type scanning electron microscope (FEI, USA)2O4The self-supporting electrode material for the negative electrode of the sodium ion battery was obtained, and as a result, it can be seen from FIG. 5 that Sb was produced2O4Self-assembling by nano-rodsArranged into flower shape and grown on the carbon cloth.
Example 4
The invention discloses a method for controllably constructing Sb based on a carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery comprises the following specific steps:
step (1): dissolving 0.74g of antimony trichloride in 40mL of deionized water to obtain an antimony solution, adjusting the pH value of the antimony solution to 5 by using a 0.6g/mL sodium hydroxide aqueous solution, carrying out anodic oxidation treatment on a carbon cloth by using 10-25 g/L ammonium dihydrogen phosphate as an electrolyte, wherein the anodic oxidation voltage is 5V, and the time is 3-7 min, and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution in the step (1) into a reaction vessel, wherein the reaction vessel is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is 10r/min, carrying out solvothermal or hydrothermal reaction for 48h at 150 ℃ in the homogeneous reactor, cooling to room temperature after the reaction is finished, taking out the carbon cloth, washing and drying to obtain the Sb controllably constructed based on the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
Example 5
The invention discloses a method for controllably constructing Sb based on a carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery comprises the following specific steps:
step (1): dissolving 0.67g of antimony trichloride in a mixed solvent of 10mL of anhydrous ethanol and 30mL of deionized water to obtain an antimony solution, adjusting the pH value of the antimony solution to 6 by using 0.6g/mL of sodium hydroxide aqueous solution, carrying out anodic oxidation treatment on carbon cloth by using 10-25 g/L of ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, and the time is 3-5 min, and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution in the step (1) into a reaction vessel, wherein the reaction vessel is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is 10r/min, carrying out solvothermal or hydrothermal reaction for 12h at 180 ℃ in the homogeneous reactor, cooling to room temperature after the reaction is finished, taking out the carbon cloth, washing and drying to obtain a baseControllable construction of Sb on carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
Example 6
The invention discloses a method for controllably constructing Sb based on a carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery comprises the following specific steps:
step (1): dissolving 0.5g of antimony trichloride in 20mL of absolute ethyl alcohol to obtain an antimony solution, adjusting the pH value of the antimony solution to 6 by using 0.6g/mL of sodium hydroxide aqueous solution, carrying out anodic oxidation treatment on carbon cloth by using 10-25 g/L of ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, and the time is 3-7 min, and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution in the step (1) into a reaction vessel, wherein the reaction vessel is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is 10r/min, carrying out solvothermal or hydrothermal reaction for 24h at 180 ℃ in the homogeneous reactor, cooling to room temperature after the reaction is finished, taking out the carbon cloth, washing and drying to obtain the Sb controllably constructed based on the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
Example 7
The invention discloses a method for controllably constructing Sb based on a carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery comprises the following specific steps:
step (1): dissolving 0.8g of antimony trichloride in a mixed solvent of 10mL of anhydrous ethanol and 20mL of deionized water to obtain an antimony solution, adjusting the pH value of the antimony solution to 7 by using 0.6g/mL of sodium hydroxide aqueous solution, carrying out anodic oxidation treatment on carbon cloth by using 10-25 g/L of ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, and the time is 3-7 min, and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution in the step (1) into a reaction vessel, wherein the reaction vessel is preferably a homogeneous reactor, the rotating speed of the homogeneous reactor is 10r/min, carrying out solvothermal or hydrothermal reaction for 24h at the temperature of 150 ℃ in the homogeneous reactor, and after the reaction is finishedCooling to room temperature, taking out the carbon cloth, washing and drying to obtain Sb controllably constructed based on the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
Example 8
The invention discloses a method for controllably constructing Sb based on a carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery comprises the following specific steps:
step (1): dissolving 0.5g of antimony trichloride in a mixed solvent of 20mL of anhydrous ethanol and 20mL of deionized water to obtain an antimony solution, adjusting the pH value of the antimony solution to 4 by using 0.6g/mL of sodium hydroxide aqueous solution, carrying out anodic oxidation treatment on carbon cloth by using 10-25 g/L of ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, and the time is 3-7 min, and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution in the step (1) into a reaction vessel, wherein the reaction vessel is preferably a homogeneous reactor, the rotation speed of the homogeneous reactor is 10r/min, carrying out solvothermal or hydrothermal reaction for 12h at 150 ℃ in the homogeneous reactor, cooling to room temperature after the reaction is finished, taking out the carbon cloth, washing and drying to obtain the Sb controllably constructed based on the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
Example 9
The invention discloses a method for controllably constructing Sb based on a carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery comprises the following specific steps:
step (1): dissolving 0.57g of antimony trichloride in 20mL of absolute ethyl alcohol pure solvent to obtain an antimony solution, adjusting the pH value of the antimony solution to 2 by using NaOH, carrying out anodic oxidation treatment on the carbon cloth by using 10-25 g/L ammonium dihydrogen phosphate as electrolyte, wherein the anodic oxidation voltage is 5V, and the time is 3-7 min, and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution in the step (1) into a reaction vessel, wherein the reaction vessel is preferably a homogeneous reactor, the rotating speed of the homogeneous reactor is 10r/min, and the reaction is carried out in the homogeneous reactor at 180 DEG CCarrying out solvothermal or hydrothermal reaction for 48h, cooling to room temperature after the reaction is finished, taking out the carbon cloth, washing and drying to obtain Sb controllably constructed based on the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
In conclusion, the invention takes absolute ethyl alcohol or deionized water as a pure solvent or a mixed solution of the absolute ethyl alcohol and the deionized water as a solvent, and SbCl3As an antimony source, Sb is controllably constructed on carbon cloth by adopting a simple one-step solvothermal or hydrothermal method without adjusting the pH value of an antimony solution or adjusting the pH value of the antimony solution by using a sodium hydroxide aqueous solution2O4Due to Sb prepared on carbon cloth2O4Has special appearance and high theoretical specific capacity, so the material shows better electrochemical performance when being used as a self-supporting cathode material of a sodium ion battery. In addition, the method has the advantages of simple process, good controllability and short preparation period, and is suitable for large-scale industrial production.

Claims (5)

1. Sb based on controllable construction of carbon cloth substrate2O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery is characterized by comprising the following specific steps of:
step (1): dissolving 0.5-0.8 g of antimony trichloride in a solvent of less than or equal to 40mL to obtain an antimony solution, wherein the solvent is one or a mixed solution of absolute ethyl alcohol and deionized water, and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution, or regulating the pH value of the antimony solution to 2-7 by using a sodium hydroxide aqueous solution and then soaking the carbon cloth subjected to anodic oxidation treatment in the antimony solution;
step (2): transferring the carbon cloth and the antimony solution obtained in the step (1) into a reaction container, carrying out solvothermal or 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, washing and drying to obtain Sb based on the controllable construction of the carbon cloth substrate2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
2. The carbon-cloth-based substrate controllable construction Sb of claim 12O4Self-supporting electrode material for sodium ion battery cathodeThe preparation method is characterized by comprising the following steps: in the step (1), 0.6g/mL of aqueous sodium hydroxide solution is used for adjusting the pH value of the antimony solution.
3. The carbon-cloth-based substrate controllable construction Sb of claim 12O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery is characterized by comprising the following steps of: the electrolyte used in the anodic oxidation treatment in the step (1) is 10-25 g/L ammonium dihydrogen phosphate, the anodic oxidation voltage is 5V, and the time is 3-7 min.
4. The carbon-cloth-based substrate controllable construction Sb of claim 12O4The preparation method of the self-supporting electrode material for the cathode of the sodium-ion battery is characterized by comprising the following steps of: the reaction vessel in the step (2) is a homogeneous reactor, and the rotating speed of the homogeneous reactor is 10 r/min.
5. Carbon cloth substrate-based controllable construction Sb prepared by the preparation method of any one of the preceding claims2O4The self-supporting electrode material is used for the negative electrode of the sodium ion battery.
CN202010939853.7A 2020-09-09 2020-09-09 Sb based on controllable construction of carbon cloth substrate2O4Self-supporting electrode material for sodium ion battery cathode and preparation method thereof Pending CN112038623A (en)

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