CN117317197A - Negative electrode material of antimony-based sodium ion battery and preparation method thereof - Google Patents

Negative electrode material of antimony-based sodium ion battery and preparation method thereof Download PDF

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CN117317197A
CN117317197A CN202311527759.0A CN202311527759A CN117317197A CN 117317197 A CN117317197 A CN 117317197A CN 202311527759 A CN202311527759 A CN 202311527759A CN 117317197 A CN117317197 A CN 117317197A
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negative electrode
antimony
electrode material
sodium ion
ion battery
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CN117317197B (en
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龚晓芳
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Hunan Loudi Huaxing Antimony Industry Co ltd
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Hunan Loudi Huaxing Antimony Industry Co ltd
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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
    • 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
    • H01M4/36—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
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • 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
    • H01M2004/026—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

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Abstract

The invention relates to the field of battery cathode materials, in particular to an antimony-based sodium ion battery cathode material and a preparation method thereof, comprising (A) x Sb 1‑x ) 2 S 3 The method comprises the steps of carrying out a first treatment on the surface of the A is a trivalent metal element; x is the molar ratio; x is 0.02-0.2, and the anode material prepared by the invention has better electrochemical performance and 200mAg ‑1 The capacity retention rate after 200 cycles in the current density and 0.01-3.0V charge and discharge test is above 95%.

Description

Negative electrode material of antimony-based sodium ion battery and preparation method thereof
Technical Field
The invention relates to the field of battery cathode materials, in particular to an antimony-based sodium ion battery cathode material and a preparation method thereof.
Background
Along with the continuous reduction of fossil fuels and the increasing of environmental pollution, the development of renewable clean energy sources such as wind energy, solar energy, tidal energy and the like is particularly important. However, these clean energy sources are easily affected by weather, regions, environment and the like, have the characteristics of discontinuity, instability and the like, and are difficult to realize stable output of a power grid, and the energy storage system is crucial for realizing efficient utilization of renewable energy sources. Among the numerous energy storage devices, sodium Ion Batteries (SIB) have the advantages of abundant resources, low price, environmental friendliness and the like, show great advantages and potential application values in the fields of large-scale energy storage and power transportation, and become pets of scientific researchers.
The cathode material is one of the key components of the sodium ion battery, and has important influence on the battery performance. Although sodium and lithium are the same main group and have similar physical and chemical properties, the radius of sodium ions is far greater than that of lithium ions, and the traditional graphite material does not have good sodium storage performance, so that the development of a novel negative electrode material suitable for sodium ion batteries is particularly important.
Disclosure of Invention
The invention aims to: aiming at the technical problems, the invention provides an antimony-based sodium ion battery anode material and a preparation method thereof.
The technical scheme adopted is as follows:
an antimony-based sodium ion battery negative electrode material comprising (A) x Sb 1-x ) 2 S 3 ；
A is a trivalent metal element;
x is the molar ratio;
x is 0.02-0.2.
Further, A is Bi.
Further, x is 0.05-0.15.
Further, x is 0.1.
Further, the (A) x Sb 1-x ) 2 S 3 Is in a three-dimensional petal shape.
Further, also include VS 2 。
Further, the VS 2 Is a laminated structure.
Further, graphene is also included.
Further, the (A) x Sb 1-x ) 2 S 3 、VS 2 The weight ratio of the graphene is 5-10:1:0.1.
the invention provides a preparation method of an antimony-based sodium ion battery anode material, which comprises the following steps:
mixing triethanolamine, ethylene glycol, A salt and antimony salt, heating to 120-140deg.C, stirring for 30-60min, rapidly adding sublimed sulfur,heating to reflux reaction for 1-2h, recovering room temperature, filtering out precipitate, cleaning, and drying to obtain (A) x Sb 1-x ) 2 S 3 Will (A) x Sb 1-x ) 2 S 3 、VS 2 Mixing with graphene oxide, placing into a quartz boat of a plasma reaction cavity, introducing hydrogen to remove gas in the reaction cavity, and reacting for 30-60min under the power of 100-300W, wherein the vacuum degree of the reaction cavity is 20-50 Pa.
The invention has the beneficial effects that:
the invention provides an antimony-based sodium ion battery anode material, which regulates and controls Sb by a cationic doping strategy 2 S 3 The crystal structure of the metal oxide semiconductor is obtained by a specific synthesis method, and the cation doped Sb with three-dimensional petal-shaped morphology is obtained 2 S 3 The introduction of Bi ligands not only promotes electron/ion transport by lowering the diffusion energy barrier, but also creates more reaction sites with the VS of the lamellar structure 2 And graphene combination to form a three-dimensional structure network constrained by nano space, so that the three-dimensional structure network has strong structural stability and ultra-fast Na + Storage kinetics and highly reversible redox reactions, intercalation of graphene by plasma (a x Sb 1-x ) 2 S 3 And VS (VS) 2 The specific surface area and the surface active site of the anode material are increased, the volume expansion of the electrode is inhibited, the cycle stability of the battery is enhanced, and the anode material prepared by the invention has better electrochemical performance and 200mAg -1 The capacity retention rate after 200 cycles in the current density and 0.01-3.0V charge and discharge test is above 95%.
Drawings
FIG. 1 shows three-dimensional petal-like structure (Bi) prepared in example 1 0.1 Sb 0.9 ) 2 S 3 SEM images of (a);
FIG. 2 is a VS produced in example 1 2 SEM images of (a);
fig. 3 is a schematic structural diagram of a sodium ion battery.
Detailed Description
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention. The technology not mentioned in the present invention refers to the prior art, and unless otherwise indicated, the following examples and comparative examples are parallel tests, employing the same processing steps and parameters.
Example 1:
an antimony-based sodium ion battery negative electrode material comprises three-dimensional petal-shaped (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And graphene, three-dimensional petal shape (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And the weight ratio of the graphene is 5:1:0.1;
VS 2 preparation method of (vanadium disulfide) referring to chinese patent CN106430306a, 15mL of ultrapure water is measured in a 50mL beaker at room temperature, 0.5g of polyvinylpyrrolidone K30 (PVP-K30) is placed in the beaker, stirred for 30 minutes at 800r/min by an electromagnetic stirrer until complete dissolution, 0.2mmol of ammonium metavanadate and 0.1mmol of thioacetamide are added to the obtained solution, stirring is continued until complete dissolution is performed, the dissolution color is deep brown, aqueous ammonia with a concentration of 12mol/L is added dropwise to adjust the pH to 9, the mixed solution is placed in a 25mL polytetrafluoroethylene liner, and the liner is placed in a high-pressure hydrothermal kettle. Naturally cooling to room temperature after reacting at 160deg.C for 15h, taking out black suspension, placing into 50ml centrifuge tube, washing with ultrapure water and absolute ethanol at 9800r/min for 6 times with centrifuge, collecting precipitate, oven drying with vacuum oven at 110deg.C under 0.1MPa for 8h, collecting product, and collecting VS (VS) figure 3 2 From which VS can be seen in the scanning electron micrograph of (C) 2 Is a laminated structure.
The preparation method of the negative electrode material of the antimony-based sodium ion battery comprises the following steps:
adding 18ml of triethanolamine, 500ml of ethylene glycol, 3.15g of bismuth chloride and 20.53g of antimony chloride into a 1L three-neck flask with a thermometer and a condenser tube, stirring to uniformly mix, heating to 130 ℃ to keep the temperature for 40min, rapidly adding 19.24g of sublimed sulfur, heating to reflux reaction for 2h, naturally cooling to room temperature, filtering out precipitate and adding the solution into a three-neck flaskCleaning three times with mixed solution of chloroform and n-hexane at volume ratio of 1:1, and drying in vacuum oven at 50deg.C for 10 hr to obtain three-dimensional petal (Bi) 0.1 Sb 0.9 ) 2 S 3 500mg (Bi) 0.1 Sb 0.9 ) 2 S 3 、100mg VS 2 Mixing with 10mg graphene oxide, placing into a quartz boat of a plasma reaction chamber, introducing hydrogen to remove gas in the reaction chamber, reacting for 60min under the power of 200W, wherein the vacuum degree of the reaction chamber is 20 Pa.
Example 2:
substantially the same as in example 1, except that the negative electrode material of the sodium-ion antimonide battery comprises three-dimensional petal-like (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And graphene, three-dimensional petal shape (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And the weight ratio of the graphene is 6:1:0.1.
example 3:
substantially the same as in example 1, except that the negative electrode material of the sodium-ion antimonide battery comprises three-dimensional petal-like (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And graphene, three-dimensional petal shape (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And the weight ratio of the graphene is 7:1:0.1.
example 4:
substantially the same as in example 1, except that the negative electrode material of the sodium-ion antimonide battery comprises three-dimensional petal-like (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And graphene, three-dimensional petal shape (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And the weight ratio of the graphene is 8:1:0.1.
example 5:
substantially the same as in example 1, except that the negative electrode material of the sodium-ion antimonide battery comprises three-dimensional petal-like (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And graphene, three-dimensional petal shape (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And the weight ratio of the graphene is 9:1:0.1.
example 6:
substantially the same as in example 1, except that the negative electrode material of the sodium-ion antimonide battery comprises three-dimensional petal-like (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And graphene, three-dimensional petal shape (Bi 0.1 Sb 0.9 ) 2 S 3 、VS 2 And the weight ratio of the graphene is 10:1:0.1.
comparative example 1:
substantially the same as in example 1, except that a commercially available Sb was used 2 S 3 (delta) instead of three-dimensional petal shape (Bi) 0.1 Sb 0.9 ) 2 S 3 。
Comparative example 2:
substantially the same as in example 1, except that VS was not added 2 。
Comparative example 3:
substantially the same as in example 1, except that commercial granular VS was used 2 (North Kernel) VS instead of lamellar structure 2 。
Comparative example 4:
substantially the same as in example 1, except that graphene was not added.
Performance test:
the anode materials prepared in examples 1 to 6 and comparative examples 1 to 4 of the present invention were used as test samples for electrochemical performance test;
the sodium ion battery is assembled by adopting a CR2032 button battery shell, and is carried out in a vacuum glove box under the protection atmosphere of high-purity argon. The prepared electrode plate, sodium plate and diaphragm are made into half-cell, then the electrochemical performance is tested, high-purity argon is used as protective atmosphere, the oxygen content and the water content are both less than 1ppm, and the preparation process is as follows:
(1) and (3) preparing slurry. 100mg of total mass were weighed according to 70:20:10, 70mg of a sample, 20mg of acetylene black as a conductive agent, and 10mg of CMC as a binder were weighed and mixed, and then the mixture was ground with an agate mortar for 90 minutes. Adding a proper amount of deionized water, and fully stirring to obtain uniform slurry;
(2) and (3) preparing an electrode plate. The obtained slurry was uniformly coated on a copper foil to a thickness of about 0.1mm, the prepared copper foil was placed in a vacuum drying oven, vacuum-dried (80 ℃ C., 10 h), and the dried whole copper foil was taken out and compacted with a roll press. The compacted copper foil is punched into a small wafer with the diameter of 14mm by a sheet punching machine, and finally the prepared electrode sheet is placed in a vacuum drying oven for drying at 90 ℃ for 8 hours to obtain the required electrode sheet;
(3) and assembling the battery. The electrode sheets were weighed in sequence and transferred into a vacuum glove box, and assembled using a button cell case of CR2032 type. The negative electrode adopts a prepared electrode slice, the counter electrode adopts a high-purity metal sodium slice, and the electrolyte adopts 1M NaClO 4 EC: dec=1: 1 (FEC is additive), the diaphragm adopts Celgard2400 to manufacture a sodium ion half cell, and finally the cell is sealed by a manual hydraulic sealing machine MSK-110. The battery assembly schematic diagram is shown in figure 2
The assembled sodium ion battery is subjected to constant current charge and discharge test on a CBT-138-320 battery test system, the cut-off voltage is 0.01-3.0V, and the current density is 200mAg -1 The initial specific capacity and the discharge capacity after 200 cycles of the sodium ion battery were respectively tested, and the results are shown in table 1:
table 1:
as can be seen from Table 1, the anode material prepared by the method has good electrochemical performance of 200mAg -1 The capacity retention rate after 200 cycles in the current density and 0.01-3.0V charge and discharge test is above 95%.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. An antimony-based sodium ion battery negative electrode material, characterized by comprising (A) x Sb 1-x ) 2 S 3 ；
A is a trivalent metal element;
x is the molar ratio;
x is 0.02-0.2.
2. The negative electrode material for an antimony-based sodium ion battery according to claim 1, wherein a is Bi.
3. The negative electrode material for an antimony-based sodium ion battery according to claim 1, wherein x is 0.05 to 0.15.
4. The negative electrode material for an antimony-based sodium ion battery according to claim 1, wherein x is 0.1.
5. The negative electrode material for an antimony-based sodium ion battery according to claim 1, wherein (a x Sb 1-x ) 2 S 3 Is in a three-dimensional petal shape.
6. The negative electrode material of an antimony-based sodium ion battery according to any one of claims 1-5, further comprising VS 2 。
7. The negative electrode material of an antimony-based sodium ion battery according to claim 6, wherein the VS 2 Is a laminated structure.
8. The negative electrode material of an antimony-based sodium ion battery according to claim 7, further comprising graphene.
9. The sodium antimonyl ion of claim 8A battery negative electrode material characterized in that (A) x Sb 1-x ) 2 S 3 、VS 2 The weight ratio of the graphene is 5-10:1:0.1.
10. a process for preparing negative electrode material of sodium ion antimonide battery as claimed in claim 8 or 9, characterized in that triethanolamine, ethylene glycol, A salt and antimony salt are mixed, heated to 120-140 ℃ and stirred for 30-60min, sublimed sulfur is added rapidly, heated to reflux reaction for 1-2h, filtered out precipitate after recovering room temperature, washed and dried to obtain (A) x Sb 1-x ) 2 S 3 Will (A) x Sb 1-x ) 2 S 3 、VS 2 Mixing with graphene oxide, placing into a quartz boat of a plasma reaction cavity, introducing hydrogen to remove gas in the reaction cavity, and reacting for 30-60min under the power of 100-300W, wherein the vacuum degree of the reaction cavity is 20-50 Pa.
CN202311527759.0A 2023-11-16 2023-11-16 Negative electrode material of antimony-based sodium ion battery and preparation method thereof Active CN117317197B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150318544A1 (en) * 2012-11-20 2015-11-05 Yau Wai Denis Yu Method for forming a reduced graphene oxide/metal sulfide composite and its use as an anode for batteries
CN106025272A (en) * 2016-06-27 2016-10-12 陕西科技大学 Flower-like structure Sb2S3 material for sodium ion battery anode and preparation method of flower-like structure Sb2S3 material
CN108695495A (en) * 2018-04-26 2018-10-23 上海工程技术大学 Redox graphene modifies antimonous sulfide cell negative electrode material
CN109546121A (en) * 2018-11-22 2019-03-29 广东工业大学 A kind of negative electrode material and preparation method thereof of lithium ion/sodium-ion battery
CN115275151A (en) * 2022-08-15 2022-11-01 西南石油大学 Vanadium disulfide/titanium carbide composite material and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150318544A1 (en) * 2012-11-20 2015-11-05 Yau Wai Denis Yu Method for forming a reduced graphene oxide/metal sulfide composite and its use as an anode for batteries
CN106025272A (en) * 2016-06-27 2016-10-12 陕西科技大学 Flower-like structure Sb2S3 material for sodium ion battery anode and preparation method of flower-like structure Sb2S3 material
CN108695495A (en) * 2018-04-26 2018-10-23 上海工程技术大学 Redox graphene modifies antimonous sulfide cell negative electrode material
CN109546121A (en) * 2018-11-22 2019-03-29 广东工业大学 A kind of negative electrode material and preparation method thereof of lithium ion/sodium-ion battery
CN115275151A (en) * 2022-08-15 2022-11-01 西南石油大学 Vanadium disulfide/titanium carbide composite material and preparation method and application thereof

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