CN110277550B - Preparation method of flexible sodium-ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms - Google Patents

Preparation method of flexible sodium-ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms Download PDF

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CN110277550B
CN110277550B CN201910548312.9A CN201910548312A CN110277550B CN 110277550 B CN110277550 B CN 110277550B CN 201910548312 A CN201910548312 A CN 201910548312A CN 110277550 B CN110277550 B CN 110277550B
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carbon cloth
ion battery
sodium ion
flexible
battery cathode
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CN110277550A (en
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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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    • 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
    • H01M4/362—Composites
    • 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
    • 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 relates to a preparation method of a flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms, which comprises the following steps of 1: reacting SbCl3Dissolving in absolute ethyl alcohol to obtain SbCl3Ethanol solution; step 2: dropping aqueous solution of NaOH into SbCl3Adding the mixture into an ethanol solution, and adjusting the pH value of the mixture to obtain a mixed solution; and step 3: dipping the activated carbon cloth in the mixed solution; and 4, step 4: transferring the impregnated carbon cloth and the mixed solution into a reaction container for hydrothermal reaction to prepare the antimony oxide/carbon cloth flexible sodium ion battery cathode material with different valence states and crystal forms. According to the invention, different valence states and different crystal forms of antimony oxide/carbon cloth flexible sodium ion battery cathode materials are respectively prepared by simply controlling the temperature of the hydrothermal reaction; the method has simple process, cheap raw materials, single crystal form of the obtained product, regular appearance, and wide application prospect as the flexible cathode of the sodium ion battery, and is beneficial to growing on a carbon cloth flexible substrate.

Description

Preparation method of flexible sodium-ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms
Technical Field
The invention belongs to the field of flexible battery electrode materials, and particularly relates to a preparation method of a flexible sodium-ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms.
Background
With the advent of various bendable, foldable, and lightweight electronic devices, such as flexible electronic displays, flexible phones, and the like, the development of lightweight and high-energy-density flexible secondary batteries has received attention from more researchers. The flexible electrode is one of the key factors in the development of high-performance flexible secondary batteries. Sodium ion batteries are abundant in sodium resources and low in price, and therefore, they are secondary batteries that are most promising for commercialization following lithium ion secondary batteries. Therefore, the research of the sodium ion flexible electrode has important significance. Materials used for flexible electrodes at present are graphene, carbon nanotubes, carbon cloth and the like. The carbon cloth has good mechanical properties and low price, so that the carbon cloth loaded with active substances is used as a flexible electrode material, which has been reported.
The metal oxide has the characteristic of high specific capacity when being used as the secondary electrode negative electrode material, and the metal oxide is generally polar oxide and is combined with the carbon cloth flexible electrode substrate more firmly, so the carbon cloth loaded metal oxide can be directly used as the sodium ion battery flexible negative electrode material. Antimony resources in China are abundant, antimony elements are located in the fifth main group and have two valence states of positive trivalent and positive pentavalent, and trivalent oxides are frequently reported as battery electrode materials. The most used method for the synthesis of antimony oxide is the wet method. Chinese patent publication nos. CN10554066A and CN1072392A relate to a method for preparing cubic antimony trioxide, which is prepared by directly hydrolyzing SbCl3 solution in alkali solution, but tartaric acid or its salt must be added to the hydrolysate as a crystal modifier. Chinese patent publication No. CN104512926A relates to a method for preparing orthorhombic antimony trioxide, which is also prepared by directly hydrolyzing SbCl3 solution in alkali solution, but triethanolamine must be added into the hydrolysate. Chinese patent publication No. CN101941737A relates to a preparation method of antimony pentoxide dry powder, which comprises mixing antimony trioxide, oxidant and water according to a certain proportion, stirring, refluxing, cooling, and adding inert porous material during the reaction process to obtain the antimony pentoxide with core-shell structure.
Therefore, an oxidant is required to be added in the process of synthesizing the pentavalent antimony oxide by a wet method, and a certain crystal transformation agent is required to be added in the synthesis of the trivalent antimony oxide with different crystal forms.
Disclosure of Invention
The invention aims to provide a flexible sodium ion battery taking antimony oxide/carbon cloth with different valence states and crystal formsThe preparation method of the cathode material comprises the step of respectively preparing orthorhombic Sb by controlling the temperature and time of hydrothermal reaction2O3Carbon cloth and cubic crystal Sb2O3Carbon cloth and Sb2O5The carbon cloth is different in valence state and crystal form antimony oxide/carbon cloth flexible sodium ion battery cathode material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms comprises the following steps:
step 1: 0.3-1.14 g of SbCl3Adding the mixture into 20-50 mL of absolute ethyl alcohol and dissolving to obtain SbCl3A solution;
step 2: SbCl conditioning with aqueous NaOH solution3The pH value of the solution is 7-12 to obtain a mixed solution;
and step 3: after the carbon cloth is activated, putting the carbon cloth into the mixed solution for dipping;
and 4, step 4: and transferring the carbon cloth and the mixed solution into a reaction container for hydrothermal reaction at 120-180 ℃ to obtain the antimony oxide/carbon cloth flexible sodium ion battery cathode material with different valence states and crystal forms.
Further, the mass concentration of the NaOH aqueous solution in the step 2 is 0.6-1.2 g/mL.
Further, the activation of the carbon cloth in the step 3 is one of anodic oxidation treatment, strong acid soaking treatment and low-temperature air oxidation treatment of the carbon cloth.
And further, after the carbon cloth is activated in the step 3, soaking the carbon cloth in the mixed solution for 20-40 min.
Further, the reaction vessel in the step 4 is a polytetrafluoroethylene kettle; transferring the carbon cloth and the mixed solution into a polytetrafluoroethylene kettle, and placing the polytetrafluoroethylene kettle in a homogeneous phase reactor for hydrothermal reaction for 4-48 h.
Further, the carbon cloth is hydrophilic carbon cloth, and the specification is 32cm by 16 cm.
The invention has the beneficial effects that:
the invention provides a preparation method of flexible sodium ion battery cathode materials of antimony oxide/carbon cloth with different valence states and crystal forms, which takes carbon cloth as a substrate and prepares the flexible sodium ion battery cathode materials of antimony oxide/carbon cloth with different valence states and crystal forms respectively by simply controlling the hydrothermal reaction temperature; the method has the advantages of simple process, cheap raw materials, single crystal form of the obtained product, regular appearance, and wide application prospect as the flexible cathode of the sodium ion battery, and is beneficial to growth on a carbon cloth flexible substrate.
Drawings
FIG. 1 shows orthorhombic Sb crystals prepared in example 12O3X-ray diffraction pattern of negative electrode material of carbon cloth flexible sodium ion battery;
FIG. 2 shows orthorhombic Sb crystals prepared in example 12O3X-ray diffraction pattern of negative electrode material of carbon cloth flexible sodium ion battery;
FIG. 3 shows the cubic Sb crystal prepared in example 22O3X-ray diffraction pattern of negative electrode material of carbon cloth flexible sodium ion battery;
FIG. 4 shows the cubic Sb crystal prepared in example 22O3X-ray diffraction pattern of negative electrode material of carbon cloth flexible sodium ion battery;
FIG. 5 shows Sb prepared in example 32O5X-ray diffraction pattern of negative electrode material of carbon cloth flexible sodium ion battery;
FIG. 6 shows Sb prepared in example 32O5X-ray diffraction pattern of negative electrode material of carbon cloth flexible sodium ion battery;
fig. 7 is a graph of electrochemical cycle performance of two valence antimony oxide/carbon cloth flexible sodium ion battery negative electrode materials prepared in example 2 and example 3.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
Example 1:
a preparation method of flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms comprises the following steps:
step 1: 0.57g of SbCl3Adding the mixture into 20mL of absolute ethyl alcohol and dissolving the mixture to obtain SbCl3A solution;
step 2: with 0.6g/mL of NSbCl conditioning with aqueous aOH solution3The pH value of the solution is 8 to obtain mixed solution;
and step 3: performing anodic oxidation treatment and activation on the carbon cloth, and then soaking the carbon cloth in the mixed solution for 30min, wherein the carbon cloth is hydrophilic carbon cloth and has the specification of 32cm by 16 cm;
and 4, step 4: transferring the carbon cloth and the mixed solution to a polytetrafluoroethylene kettle, placing the kettle in a homogeneous reactor, and carrying out hydrothermal reaction for 24 hours at 120 ℃ to obtain the orthorhombic Sb2O3A carbon cloth flexible sodium ion battery cathode material.
As shown in FIG. 1, orthorhombic Sb was analyzed by a Nippon Denko K.sub.max 2000 PCX-ray diffractometer2O3The negative electrode material of the/carbon cloth flexible sodium ion battery is found in the sample and Sb with the PDF number of 11-06892O3The structure is consistent, and characteristic peaks appear at 25.47 degrees, 28.38 degrees, 28.61 degrees, 43.96 degrees and 50.44 degrees. As shown in FIG. 2, the sample was observed for morphology by using a field emission scanning electron microscope (FEI, USA S-4800 type), and the obtained orthorhombic Sb crystal was observed2O3The particles are blocky and have larger sizes, and are dispersedly grown on the carbon cloth.
Example 2:
a preparation method of flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms comprises the following steps:
step 1: 1.14g of SbCl3Adding the mixture into 40mL of absolute ethyl alcohol and dissolving the mixture to obtain SbCl3A solution;
step 2: SbCl was adjusted with 1.2g/mL aqueous NaOH3The pH value of the solution is 10 to obtain mixed solution;
and step 3: performing anodic oxidation treatment and activation on the carbon cloth, and then soaking the carbon cloth in the mixed solution for 30min, wherein the carbon cloth is hydrophilic carbon cloth and has the specification of 32cm by 16 cm;
and 4, step 4: transferring the carbon cloth and the mixed solution to a polytetrafluoroethylene kettle, placing the kettle in a homogeneous reactor, and carrying out hydrothermal reaction for 24 hours at 150 ℃ to obtain cubic crystal Sb2O3A carbon cloth flexible sodium ion battery cathode material.
As shown in FIG. 3, cubic Sb crystals were analyzed by a Japanese Denko D/max2000 PCX-ray diffractometer2O3The negative electrode material of the/carbon cloth flexible sodium ion battery is found in the sample and Sb with the PDF number of 43-10712O3The structures are consistent, and characteristic peaks appear at 27.69 degrees, 32.08 degrees, 35.05 degrees, 46.00 degrees and 54.54 degrees. As shown in FIG. 4, the sample was observed for morphology by using a field emission scanning electron microscope of type S-4800 FEI, USA, and cubic crystal Sb was observed2O3Are spherical particles and grow on the carbon cloth tightly.
Example 3:
a preparation method of flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms comprises the following steps:
step 1: 0.57g of SbCl3 was added to 20mL of absolute ethanol and dissolved to obtain SbCl3A solution;
step 2: SbCl was adjusted with 0.6g/mL aqueous NaOH3The pH value of the solution is 9 to obtain mixed solution;
and step 3: soaking the carbon cloth in the mixed solution for 40min after anodic oxidation treatment and activation, wherein the carbon cloth is hydrophilic carbon cloth and has the specification of 32cm by 16 cm;
and 4, step 4: transferring the carbon cloth and the mixed solution to a polytetrafluoroethylene kettle, placing the kettle in a homogeneous phase reactor, and carrying out hydrothermal reaction for 24 hours at 180 ℃ to obtain Sb2O5A carbon cloth flexible sodium ion battery cathode material.
As shown in FIG. 5, orthorhombic Sb was analyzed by a Nippon Denko K.sub.max 2000 PCX-ray diffractometer2O3The negative electrode material of the/carbon cloth flexible sodium ion battery is found in the sample and Sb with the PDF number of 11-06902O3The structure is consistent, and characteristic peaks appear at 14.87 degrees, 28.70 degrees, 30.00 degrees, 34.78 degrees, 50.05 degrees and 59.47 degrees. As shown in FIG. 6, the sample was observed for morphology using a field emission scanning electron microscope (FEI, USA S-4800 type), and Sb was observed2O5Are spherical particles, and are uniformly grown on the carbon cloth as a monomolecular layer, and the diameter of the monomolecular layer is about 50 nm.
As shown in FIG. 7, the cubic form Sb prepared in example 2 and example 3 was crystallized2O3Carbon cloth and Sb2O5Respectively assembling carbon cloth flexible sodium ion battery cathode materialsCR2032 type button cell, and constant current charge-discharge cycle performance test is carried out on a blue test system, and the result is found to be 100mA-1Shows stable specific charge-discharge capacity under current density, wherein Sb2O5Cubic crystal Sb of/carbon cloth ratio2O3The carbon cloth used as the negative electrode material of the sodium ion battery shows higher specific discharge capacity, and when the material is circulated to 20 circles, the specific discharge capacity is 1500mAh-1And 500mAh.g-1。
Example 4:
a preparation method of flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms comprises the following steps:
step 1: 0.3g of SbCl3Adding the mixture into 20mL of absolute ethyl alcohol and dissolving the mixture to obtain SbCl3A solution;
step 2: SbCl was adjusted with 0.6g/mL aqueous NaOH3The pH value of the solution is 11 to obtain mixed solution;
and step 3: performing anodic oxidation treatment and activation on the carbon cloth, and then soaking the carbon cloth in the mixed solution for 30min, wherein the carbon cloth is hydrophilic carbon cloth and has the specification of 32cm by 16 cm;
and 4, step 4: transferring the carbon cloth and the mixed solution to a polytetrafluoroethylene kettle, placing the kettle in a homogeneous reactor, and performing hydrothermal reaction for 12 hours at 120 ℃ to obtain orthorhombic Sb2O3A carbon cloth flexible sodium ion battery cathode material.
Analysis of orthorhombic Sb by means of Nippon science D/max2000 PCX-ray diffractometer2O3The negative electrode material of the/carbon cloth flexible sodium ion battery is found in the sample and Sb with the PDF number of 11-06892O3The structure is consistent, and characteristic peaks appear at 25.47 degrees, 28.38 degrees, 28.61 degrees, 43.96 degrees and 50.44 degrees.
Example 5:
a preparation method of flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms comprises the following steps:
step 1: 1.14g of SbCl3Adding the mixture into 50mL of absolute ethyl alcohol and dissolving the mixture to obtain SbCl3A solution;
step 2: SbCl was adjusted with 0.7g/mL aqueous NaOH3The pH value of the solution is 10 to obtain mixed solution;
and step 3: performing anodic oxidation treatment and activation on the carbon cloth, and then soaking the carbon cloth in the mixed solution for 30min, wherein the carbon cloth is hydrophilic carbon cloth and has the specification of 32cm by 16 cm;
and 4, step 4: transferring the carbon cloth and the mixed solution to a polytetrafluoroethylene kettle, placing the kettle in a homogeneous phase reactor, and performing hydrothermal reaction for 10 hours at 150 ℃ to obtain cubic crystal Sb2O3A carbon cloth flexible sodium ion battery cathode material.
Analysis of cubic Sb crystals by means of a Japan science D/max2000 PCX-ray diffractometer2O3The negative electrode material of the/carbon cloth flexible sodium ion battery is found in the sample and Sb with the PDF number of 43-10712O3The structures are consistent, and characteristic peaks appear at 27.69 degrees, 32.08 degrees, 35.05 degrees, 46.00 degrees and 54.54 degrees.
Example 6:
a preparation method of flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms comprises the following steps:
step 1: 0.57g of SbCl3Adding the mixture into 20mL of absolute ethyl alcohol and dissolving the mixture to obtain SbCl3A solution;
step 2: SbCl was adjusted with 1g/mL aqueous NaOH3The pH value of the solution is 12 to obtain mixed solution;
and step 3: soaking and activating carbon cloth with strong acid, and soaking in the mixed solution for 30min, wherein the carbon cloth is hydrophilic carbon cloth and has specification of 32cm x 16 cm;
and 4, step 4: transferring the carbon cloth and the mixed solution to a polytetrafluoroethylene kettle, placing the kettle in a homogeneous phase reactor, and carrying out hydrothermal reaction for 48 hours at 180 ℃ to obtain Sb2O5A carbon cloth flexible sodium ion battery cathode material.
Analysis of Sb by means of Japanese science D/max2000 PCX-ray diffractometer2O5The negative electrode material of the/carbon cloth flexible sodium ion battery is found in the sample and Sb with the PDF number of 11-06902O5The structure is consistent, and characteristic peaks appear at 14.87 degrees, 28.70 degrees, 30.00 degrees, 34.78 degrees, 50.05 degrees and 59.47 degrees.
Example 7:
a preparation method of flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms comprises the following steps:
step 1: 0.3g of SbCl3Adding the mixture into 30mL of absolute ethyl alcohol and dissolving the mixture to obtain SbCl3A solution;
step 2: SbCl was adjusted with 0.8g/mL aqueous NaOH3The pH value of the solution is 7 to obtain mixed solution;
and step 3: soaking the carbon cloth in the mixed solution for 30min after low-temperature air oxidation activation, wherein the carbon cloth is hydrophilic carbon cloth and has the specification of 32cm by 16 cm;
and 4, step 4: transferring the carbon cloth and the mixed solution to a polytetrafluoroethylene kettle, placing the kettle in a homogeneous phase reactor, and carrying out hydrothermal reaction for 4 hours at 180 ℃ to obtain orthorhombic Sb2O5A carbon cloth flexible sodium ion battery cathode material.
Analysis of Sb by means of Japanese science D/max2000 PCX-ray diffractometer2O5The negative electrode material of the/carbon cloth flexible sodium ion battery is found in the sample and Sb with the PDF number of 11-06902O5The structure is consistent, and characteristic peaks appear at 25.47 degrees, 28.38 degrees, 28.61 degrees, 43.96 degrees and 50.44 degrees.
Example 8:
a preparation method of flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms comprises the following steps:
step 1: 1.14g of SbCl3Adding the mixture into 35mL of absolute ethyl alcohol and dissolving the mixture to obtain SbCl3A solution;
step 2: SbCl was adjusted with 0.9g/mL aqueous NaOH3The pH value of the solution is 10 to obtain mixed solution;
and step 3: performing anodic oxidation treatment and activation on the carbon cloth, and then soaking the carbon cloth in the mixed solution for 30min, wherein the carbon cloth is hydrophilic carbon cloth and has the specification of 32cm by 16 cm;
and 4, step 4: transferring the carbon cloth and the mixed solution to a polytetrafluoroethylene kettle, placing the kettle in a homogeneous reactor, and carrying out hydrothermal reaction for 36 hours at 120 ℃ to obtain orthorhombic Sb2O3A carbon cloth flexible sodium ion battery cathode material.
Analysis of orthorhombic crystals by means of the Japanese science D/max2000 PCX-ray diffractometerSb2O3The negative electrode material of the/carbon cloth flexible sodium ion battery is found in the sample and Sb with the PDF number of 11-06892O3The structure is consistent, and characteristic peaks appear at 25.47 degrees, 28.38 degrees, 28.61 degrees, 43.96 degrees and 50.44 degrees.
In a word, the invention takes carbon cloth as a substrate, and prepares the orthorhombic Sb by simply controlling the hydrothermal reaction temperature2O3Carbon cloth and cubic crystal Sb2O3Carbon cloth and Sb2O5The carbon cloth is different in valence state and crystal form antimony oxide/carbon cloth flexible sodium ion battery cathode material. The preparation method of the different-valence antimony oxide/carbon cloth flexible sodium ion battery cathode material provided by the invention has the advantages of simple process, cheap raw materials, single crystal form of the obtained product, regular appearance, and wide application prospect as the flexible cathode of the sodium ion battery, and is beneficial to growth on a carbon cloth flexible substrate.

Claims (1)

1. A preparation method of flexible sodium ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms is characterized by comprising the following steps:
step 1: 0.3-1.14 g of SbCl3Adding the mixture into 20-50 mL of absolute ethyl alcohol and dissolving to obtain SbCl3A solution;
step 2: SbCl conditioning with aqueous NaOH solution3The pH value of the solution is 10-12 to obtain a mixed solution; the mass concentration of the NaOH aqueous solution is 0.6-1.2 g/mL;
and step 3: after the carbon cloth is activated, putting the carbon cloth into the mixed solution for dipping; the carbon cloth is hydrophilic carbon cloth with the specification of 32cm by 16 cm; the activation of the carbon cloth is one of anodic oxidation treatment, strong acid soaking treatment and low-temperature air oxidation treatment of the carbon cloth; immersing the activated carbon cloth in the mixed solution for 20-40 min;
and 4, step 4: transferring the carbon cloth and the mixed solution into a polytetrafluoroethylene kettle, placing the kettle in a homogeneous reactor, and carrying out hydrothermal reaction at 120 ℃ to obtain orthorhombic Sb2O3A carbon cloth flexible sodium ion battery cathode material; carrying out hydrothermal reaction at 150 ℃ to obtain cubic crystal Sb2O3A carbon cloth flexible sodium ion battery cathode material; at 180 deg.C under waterThermal reaction to obtain Sb2O5A carbon cloth flexible sodium ion battery cathode material.
CN201910548312.9A 2019-06-24 2019-06-24 Preparation method of flexible sodium-ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms Active CN110277550B (en)

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