CN114613958B - Material used as negative electrode of sodium ion battery and preparation method thereof - Google Patents

Material used as negative electrode of sodium ion battery and preparation method thereof Download PDF

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CN114613958B
CN114613958B CN202210251608.6A CN202210251608A CN114613958B CN 114613958 B CN114613958 B CN 114613958B CN 202210251608 A CN202210251608 A CN 202210251608A CN 114613958 B CN114613958 B CN 114613958B
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蔡玉荣
樊润泽
赵陈煜
马佳慧
陆子枫
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Zhejiang Sci Tech University ZSTU
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—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
    • H01M4/58—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
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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
    • 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
    • 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
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a material used as a negative electrode of a sodium ion battery and a preparation method thereof, and the preparation method of the material used as the negative electrode of the sodium ion battery comprises the following steps: sequentially and slowly adding ammonium metavanadate, ammonia water and bismuth nitrate pentahydrate into continuously stirred deionized water, transferring the mixed solution into a 50ml liner, performing hydrothermal reaction, performing suction filtration, washing and drying to obtain VBiO 4 Precursor, VBiO 4 The precursor is subjected to Dopamine (DA) in-situ polymerization coating to obtain VBiO 4 PDA, VBiO 4 Mixing @ PDA with sulfur powder, and vulcanizing in a nitrogen atmosphere of a tube furnace to obtain VS 4 /Bi 2 S 3 The @ PDA heterojunction nanorod is used as a negative electrode material of a sodium ion battery. The invention belongs to the technical field of new energy, and provides a material used as a negative electrode of a sodium ion battery and a preparation method thereof.

Description

Material used as negative electrode of sodium ion battery and preparation method thereof
Technical Field
The invention belongs to the technical field of new energy, and particularly relates to a material used as a negative electrode of a sodium ion battery and a preparation method thereof.
Background
For many years, due to serious environmental pollution and energy crisis, advanced energy shortage technology has attracted widespread attention, lithium ion batteries are ubiquitous energy storage devices in our daily life, but the disadvantages of low lithium reserves, uneven regional distribution and the like limit the application of the lithium ion batteries, because of abundant sodium resources in the global scope and similar charge storage mechanisms as those of the lithium ion batteries, sodium ion batteries are the most promising alternatives, however, the larger radius and heavier molar mass of sodium ions lead to slow reaction kinetics and remarkable volume change of electrode materials, thereby leading to poor rate performance and high irreversible capacity loss of the sodium ion batteries, and therefore, development of electrode materials suitable for the sodium ion batteries is imperative.
In the negative electrode of the sodium ion battery, the conversion metal sulfide such as MSx, M= V, mo, ni, cu and the like which is recently widely focused obtains higher theoretical specific capacity due to the intrinsic property of multi-electron transfer, so that the material becomes a negative electrode material of the sodium ion battery with great potential at present, but the practical application of the material in the sodium ion battery is hindered by the poor multiplying power capacity and short cycle life of MSx.
In order to solve the problems, researchers carry out a series of modifications on the cathode material, such as modification of carbon coating surface engineering to improve the conductivity of the active material and maintain the structural stability of the material, and the nanostructure design regulates and controls the microstructure evolution of the material in the charge and discharge process, so as to improve the rate capability and the cycle life. The methods increase the structural stability of the material to a certain extent, but can not change the intrinsic characteristics of the active material and can not improve the migration rate of Na+, so that the rate performance and the sodium storage capacity of the battery can not be obviously improved, and based on the method, we can realize the VS (VS) 4 Incorporation of Bi into a substrate 2 S 3 Constructing a heterostructure, effectively improving the intrinsic electron migration rate, enhancing the reaction kinetics, further effectively improving the multiplying power performance and sodium storage capacity, and then carrying out carbon coating on the heterostructure to keep the structural stability of the material and improve the conductivity, wherein in the field of preparation of negative electrode materials of sodium ion batteries, a cobalt-doped vanadium disulfide micron sheet and a preparation method thereof are disclosed in China patent (CN 113193198A), and the micron sheet of cobalt-doped vanadium disulfide is prepared by a solvothermal method and is used as the negative electrode material of the sodium ion batteries; chinese patent (CN 111584847B) is a vanadium disulfide and black phosphorus composite electrode material and a preparation method thereof, wherein the black phosphorus is firstly stripped, the vanadium disulfide is secondly stripped, and the most isThen compounding vanadium disulfide and black phosphorus to obtain a vanadium disulfide and black phosphorus composite electrode material; chinese patent (CN 109888223B) relates to a preparation method and application of vanadium tetrasulfide@reduced graphene oxide composite powder, wherein the vanadium tetrasulfide@reduced graphene oxide composite powder is obtained by in-situ growth by a hydrothermal method and is used as an electrode material, and according to the current investigation situation, the application of the vanadium tetrasulfide@reduced graphene oxide composite powder in VS is not seen yet 4 Incorporation of Bi into a substrate 2 S 3 The heterostructure is constructed, carbon coating is carried out on the heterostructure, and the heterostructure is used as a negative electrode material of a sodium ion battery and a preparation method of the heterostructure, so that the defects of poor multiplying power capacity, short cycle life and the like of a vanadium-based sulfide in the sodium ion battery are overcome.
Disclosure of Invention
Aiming at the situation, the invention aims to overcome the defects of the prior art and provide a material used as a negative electrode of a sodium ion battery and a preparation method thereof, and the method is simple and convenient to operate and low in cost.
Another object of the present invention is to provide a material for negative electrode of sodium ion battery, which is prepared by the above preparation method, and has low cost and excellent performance.
The invention finally aims to provide the application of the material used as the negative electrode of the sodium ion battery, which has high specific capacity, high charge and discharge speed and long cycle life.
The technical scheme adopted by the invention is as follows: a method for preparing a material for use as a negative electrode of a sodium ion battery, comprising the steps of:
step (1): sequentially and slowly adding ammonium metavanadate, ammonia water and bismuth nitrate pentahydrate into continuously stirred deionized water to obtain a mixed solution with better dispersion;
step (2): transferring the mixed solution with better dispersion in the step (1) into a 50ml lining, and obtaining a hydrothermal product through hydrothermal reaction;
step (3): filtering, washing and drying the hydrothermal product in the step (2) to obtain VBiO 4 A precursor;
step (4): VBiO in the step (3) 4 The precursor is subjected to Dopamine (DA) in-situ polymerization coating to obtain VBiO 4 @PDA；
Step (5): VBiO in the step (4) 4 Mixing @ PDA with sulfur powder, and vulcanizing in a nitrogen atmosphere of a tube furnace to obtain VS 4 /Bi 2 S 3 The @ PDA heterojunction nanorod is used as a negative electrode material of a sodium ion battery.
Further, the molar ratio of bismuth nitrate pentahydrate to ammonium metavanadate in the step (1) is 1:2-6, and the ammonia water is 1-3 ml.
Still further, the continuous stirring time in the step (1) is 150-210 min, and the deionized water is 25-35 ml.
Wherein the hydrothermal reaction temperature in the step (2) is 160-200 ℃ and the reaction time is 18-22 h.
In addition, the drying temperature in the step (3) is 60-80 ℃.
Preferably, the mass ratio of the dopamine hydrochloride (DA.HCl) to the precursor VBiO4 in the step (4) is 1:2-4.
Finally, step (5) the VS 4 /Bi 2 S 3 The mixing mass ratio of the @ PDA and the sulfur powder is 1:25-35, and the vulcanization temperature is 500-700 ℃.
The invention also provides the VS prepared by the preparation method 4 /Bi 2 S 3 Negative electrode material of @ PDA heterojunction nanorod battery and VS 4 /Bi 2 S 3 Application of anode material of PDA heterojunction nanorod battery in preparing sodium ion battery.
After the technical scheme is adopted, the invention has the following beneficial effects: compared with the prior art, the preparation process is simple, quick and efficient, and the prepared VS 4 /Bi 2 S 3 The anode material of the PDA heterojunction nanorod battery has high specific capacity, good conductivity, electrochemical activity and cycling stability, and is particularly suitable for manufacturing the anode of a sodium ion battery.
Drawings
FIG. 1 is VBiO prepared in example 1 4 A field emission Scanning Electron Microscope (SEM) photograph of the precursor.
FIG. 2 is a VS prepared in example 1 4 /Bi 2 S 3 Field emission Scanning Electron Microscope (SEM) photographs of PDA heterojunction nanorods.
FIG. 3 is a real worldVS prepared in example 1 4 /Bi 2 S 3 The @ PDA heterojunction nanorod electrode material is used as a negative electrode material of a sodium ion battery at 2A g -1 Long cycle performance plot for 1000 cycles of current density.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1 0.002mol of ammonium metavanadate was first dispersed in 30ml of deionized water while slowly adding 2ml of ammonia water with continuous stirring, then 0.0005mol of bismuth nitrate pentahydrate was added to the above solution, stirred for 180min, finally a uniform yellow solution was obtained, transferred to a 50ml polytetrafluoroethylene-lined sealed autoclave, and reacted at 180 c for 20h. Cooling to room temperature, washing the hydrothermal product with deionized water and ethanol for several times, and drying in a forced air drying oven at 60deg.C for 12 hr to obtain precursor VBiO 4 Yellow powder. 50mg of VBiO prepared 4 The nanorods were dispersed in Tris buffer (10 Mmol,50 mL) and sonicated for 2h, then 25mg dopamine hydrochloride (DA. HCl) was added to the solution and stirred vigorously for 6h. Black VBiO was collected by rinsing with deionized water several times and drying 4 PDA powder. Then the prepared 50mg VBiO is added 4 The @ PDA nanorods and 1.5g of sublimed sulfur were mixed together in a crucible. Finally, in the tube furnace N 2 Vulcanizing for 4 hours at 600 ℃ in the atmosphere to obtain VS 4 /Bi 2 S 3 @ PDA composite. Prepared VS 4 /Bi 2 S 3 Mixing the anode material of the PDA battery, ketjen black and polyvinylidene fluoride (PVDF) in a mass ratio of 7:2:1 in an N-methyl-2-pyrrolidone (NMP) solvent, mixing and stirring to obtain uniform slurry, smearing the uniform slurry on a copper foil current collector, and drying the uniform slurry in a vacuum oven at 120 ℃ for overnight. Cooling to room temperature, taking out slices, weighing, putting into a glove box, balancing for 24 hours, assembling into a sodium ion battery, and testing the electrochemical property of the batteryCan be used.
Example 2 first 0.002mol of ammonium metavanadate was dispersed in 25ml of deionized water while slowly adding 1ml of ammonia water with continuous stirring, then 0.001mol of bismuth nitrate pentahydrate was added to the above solution, stirred for 150min, finally a uniform yellow solution was obtained, transferred to a 50ml polytetrafluoroethylene-lined sealed autoclave, and reacted at 200 c for 18h. Cooling to room temperature, washing the hydrothermal product with deionized water and ethanol for several times, and drying in a forced air drying oven at 70deg.C for 12 hr to obtain precursor VBiO 4 Yellow powder. 100mg of VBiO prepared 4 The nanorods were dispersed in Tris buffer (10 Mmol,50 mL) and sonicated for 2h, then 25mg dopamine hydrochloride (DA. HCl) was added to the solution and stirred vigorously for 6h. Black VBiO was collected by rinsing with deionized water several times and drying 4 PDA powder. Then the prepared 50mgVBiO 4 The @ PDA nanorods and 1.25g of sublimed sulfur were mixed together in a crucible. Finally, in the tube furnace N 2 Vulcanizing for 4 hours at 500 ℃ in atmosphere to obtain VS 4 /Bi 2 S 3 @ PDA composite. Prepared VS 4 /Bi 2 S 3 Mixing the anode material of the PDA battery, ketjen black and polyvinylidene fluoride (PVDF) in a mass ratio of 7:2:1 in an N-methyl-2-pyrrolidone (NMP) solvent, mixing and stirring to obtain uniform slurry, smearing the uniform slurry on a copper foil current collector, and drying the uniform slurry in a vacuum oven at 120 ℃ for overnight. And cooling to room temperature, taking out slices, weighing, putting into a glove box, balancing for 24 hours, assembling into a sodium ion battery, and testing the electrochemical performance of the battery.
Example 3 0.0018mol of ammonium metavanadate was first dispersed in 35ml of deionized water while slowly adding 3ml of ammonia with continuous stirring, then 0.0003mol of bismuth nitrate pentahydrate was added to the above solution, stirred for 210min, finally a homogeneous yellow solution was obtained, transferred to a 50ml polytetrafluoroethylene-lined sealed autoclave, and reacted at 160 deg.c for 22h. Cooling to room temperature, washing the hydrothermal product with deionized water and ethanol for several times, and drying in a forced air drying oven at 80deg.C for 12 hr to obtain precursor VBiO 4 Yellow powder. 75mg of VBiO prepared 4 The nanorods were dispersed into Tris buffer (10 Mmol,50 mL) and sonicated for 2h, followed by25mg of dopamine hydrochloride (DA. HCl) are added to the solution and stirred vigorously for 6h. Black VBiO was collected by rinsing with deionized water several times and drying 4 PDA powder. Then the prepared 50mgVBiO 4 The @ PDA nanorods and 1.75g of sublimed sulfur were mixed together in a crucible. Finally, in the tube furnace N 2 Vulcanizing for 4 hours at 700 ℃ in the atmosphere to obtain VS 4 /Bi 2 S 3 @ PDA composite. Prepared VS 4 /Bi 2 S 3 Mixing the anode material of the PDA battery, ketjen black and polyvinylidene fluoride (PVDF) in a mass ratio of 7:2:1 in an N-methyl-2-pyrrolidone (NMP) solvent, mixing and stirring to obtain uniform slurry, smearing the uniform slurry on a copper foil current collector, and drying the uniform slurry in a vacuum oven at 120 ℃ for overnight. And cooling to room temperature, taking out slices, weighing, putting into a glove box, balancing for 24 hours, assembling into a sodium ion battery, and testing the electrochemical performance of the battery.
The three VSs prepared in examples 1, 2 and 3 were measured 4 /Bi 2 S 3 Anode material of PDA battery at 2A g -1 Electrochemical performance at current density. Table 1 shows the VSs prepared in examples 1, 2 and 3 4 /Bi 2 S 3 Characterization results of PDA cell negative electrode material. As can be seen from the data in Table 1, VS obtained by the preparation method of the present invention 4 /Bi 2 S 3 Anode materials (a), (b) and (c) of PDA battery are 2A g -1 The 1000 circles of the high-current density still show 473.416mAh g -1 、458.245mAh g -1 、430.487mAh g -1 Excellent sodium storage performance.
As shown in FIG. 2, VS prepared from example 1 4 /Bi 2 S 3 The morphology of the field emission scanning electron microscope photo of the anode material of the PDA battery is nano rod.
TABLE 1
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
The invention and its embodiments have been described above without limitation, and the actual construction is not limited thereto. In summary, if one of ordinary skill in the art is informed by this disclosure, a structural manner and an embodiment similar to the technical solution should not be creatively devised without departing from the gist of the present invention.

Claims (1)

1.VS 4 /Bi 2 S 3 Application of anode material of PDA heterojunction nanorod battery in preparing sodium ion battery to improve sodium storage performance;
the VS 4 /Bi 2 S 3 The preparation method of the anode material of the PDA heterojunction nanorod battery comprises the following steps:
step (1): sequentially and slowly adding ammonium metavanadate, ammonia water and bismuth nitrate pentahydrate into continuously stirred deionized water to obtain a mixed solution with better dispersion; the molar ratio of the bismuth nitrate pentahydrate to the ammonium metavanadate is 1:4, and the ammonia water is 2ml; the continuous stirring time is 180min, and the deionized water is 30ml;
step (2): transferring the mixed solution with better dispersion in the step (1) into a 50ml lining, and obtaining a hydrothermal product through hydrothermal reaction; the hydrothermal reaction temperature is 180 ℃ and the reaction time is 20 hours;
step (3): filtering, washing and drying the hydrothermal product in the step (2) to obtain VBiO 4 A precursor; the drying temperature is 60 ℃ and the drying time is 12 hours;
step (4): VBiO in the step (3) 4 The precursor is subjected to dopamine in-situ polymerization coating to obtain VBiO 4 A @ PDA; dopamine hydrochloride and precursor VBiO 4 The mass ratio is 1:2;
step (5): VBiO in the step (4) 4 Mixing @ PDA with sulfur powder, and vulcanizing in a nitrogen atmosphere of a tube furnace to obtain VS 4 /Bi 2 S 3 The @ PDA heterojunction nanorod is used as a negative electrode material of the sodium ion battery; the VBiO 4 The mass ratio of the @ PDA to the sulfur powder is 1:30, the vulcanization temperature is 600 ℃, and the vulcanization time is 4 hours.
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CN112599770A (en) * 2021-03-04 2021-04-02 湖南镕锂新材料科技有限公司 Lithium/sodium ion battery negative electrode material and preparation method thereof
CN113998739A (en) * 2021-03-26 2022-02-01 浙江理工大学 Preparation method of sodium ion battery negative electrode material
CN113877632A (en) * 2021-11-16 2022-01-04 江西省科学院应用化学研究所 Preparation method of 2D bismuth vanadate @ PDA core-shell structure composite material loaded with noble metal nanoparticles
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