CN115057480A - Multi-transition metal lithium-sulfur battery positive electrode material and preparation method and application thereof - Google Patents

Multi-transition metal lithium-sulfur battery positive electrode material and preparation method and application thereof Download PDF

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CN115057480A
CN115057480A CN202210977790.3A CN202210977790A CN115057480A CN 115057480 A CN115057480 A CN 115057480A CN 202210977790 A CN202210977790 A CN 202210977790A CN 115057480 A CN115057480 A CN 115057480A
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transition metal
sulfur battery
lithium
positive electrode
electrode material
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吴福根
甘甜
林志萍
王金
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Guangdong University of Technology
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    • C01G51/00—Compounds of cobalt
    • C01G51/006—Compounds containing, besides cobalt, two or more other elements, with the exception of oxygen or hydrogen
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    • C01—INORGANIC CHEMISTRY
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    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
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    • H—ELECTRICITY
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    • 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
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0404—Methods of deposition of the material by coating on electrode collectors
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • 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
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    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties

Abstract

The invention discloses a multi-transition metal lithium-sulfur battery positive electrode material and a preparation method and application thereof, and belongs to the technical field of lithium-sulfur batteries. The preparation method of the multi-transition metal lithium-sulfur battery positive electrode material comprises the following steps: adding two transition metal salts and thiourea into the graphene oxide dispersion liquid, uniformly stirring, and carrying out hydrothermal reaction to obtain the graphene oxide dispersion liquidThe multi-element transition metal lithium-sulfur battery positive electrode material is provided. In the multi-transition metal lithium-sulfur battery anode material prepared by the invention, the contained multi-transition metal sulfide has various active sites, so that Li is enhanced 2 S 8 、Li 2 S 6 、Li 2 S 4 And the multi-element transition metal compound can also enhance the electrocatalytic activity by lowering the potential barrier so as to accelerate the electrochemical conversion, and the battery prepared by adopting the battery anode material has stable cycle performance.

Description

Multi-transition metal lithium-sulfur battery positive electrode material and preparation method and application thereof
Technical Field
The invention relates to the technical field of lithium-sulfur batteries, in particular to a multi-transition metal lithium-sulfur battery positive electrode material and a preparation method and application thereof.
Background
At present, the demand of high-performance secondary batteries is continuously increased, and the energy density of the traditional lithium ion battery reaches the limit, so that the requirements of people are difficult to meet. Therefore, there is a need to develop a new secondary battery having higher energy and power density and longer cycle life. Among the new secondary battery systems, lithium-sulfur batteries have very high theoretical specific capacity (1675 mAh g) -1 ) And theoretical energy density (2600 Wh kg) -1 ) And the advantages of rich sulfur storage, low price, environmental friendliness and the like of active substances are considered to be one of the most potential high-efficiency energy storage devices in the next generation.
However, the practical application of lithium-sulfur batteries is severely restricted by the existence of various problems such as poor conductivity of sulfur and its discharge products, nearly 80% volume expansion of the positive electrode material during the charge and discharge processes, and the "shuttle effect" of the intermediate lithium polysulfide. Therefore, the search and development of suitable sulfur cathode materials to alleviate the above problems are key to overcoming the difficulties, and are a hot spot and difficulty of research.
Disclosure of Invention
The invention aims to provide a multi-element transition metal lithium sulfur battery positive electrode material, and a preparation method and application thereof, so as to solve the problems in the prior art, and the pure-phase FeCoS prepared by the method 2 the/rGO composite material can effectively solve the problem of poor lithium-sulfur battery cyclicity caused by shuttle effect and poor electron/ion conductivity of elemental sulfur in the charging and discharging processes of the lithium-sulfur battery.
In order to achieve the purpose, the invention provides the following scheme:
one of the technical schemes of the invention is as follows: a preparation method of a multi-transition metal lithium-sulfur battery positive electrode material comprises the following steps: adding two transition metal salts and thiourea into the graphene oxide dispersion liquid, uniformly stirring, and carrying out hydrothermal reaction to obtain the multi-element transition metal lithium-sulfur battery cathode material.
Further, the preparation of the graphene oxide dispersion specifically comprises: adding graphene oxide into ethylene glycol, and performing ultrasonic dispersion for 1-3 hours to obtain the graphene oxide dispersion liquid.
Further, the transition metal salt comprises iron salt and cobalt salt; the molar ratio of the ferric salt to the cobalt salt to the thiourea is 1:1: 2; the stirring time is 1-2 h; the temperature of the hydrothermal reaction is 200 ℃ and the time is 12 h.
Further, the ratio of the iron salt, the cobalt salt, the thiourea and the graphene oxide is 1 mmol: 1 mmol: 2 mmol: 50-100 mg.
The second technical scheme of the invention is as follows: multi-element transition metal lithium sulfur battery positive electrode material (FeCoS) prepared by preparation method 2 a/rGO composite).
FeCoS 2 Multi-transition metal sulfide FeCoS in/rGO composite material 2 The graphene is a single phase, uniformly grows on the laminated graphene sheet, and has excellent electrochemical performance.
The third technical scheme of the invention is as follows: an application of the multi-transition metal lithium-sulfur battery positive electrode material in the preparation of a lithium-sulfur battery.
The fourth technical scheme of the invention is as follows: a positive plate of a lithium-sulfur battery comprises a current collector and a coating layer coated on the surface of the current collector; the coating layer comprises the multi-element transition metal lithium-sulfur battery cathode material.
The fifth technical scheme of the invention is as follows: the preparation method of the positive plate of the lithium-sulfur battery comprises the following steps:
and mixing and stirring the multi-element transition metal lithium-sulfur battery positive electrode material, sulfur powder, carbon black and a binder to prepare slurry, uniformly coating the slurry on a current collector, and drying to obtain the lithium-sulfur battery positive electrode plate.
Further, the mass ratio of the multi-element transition metal lithium-sulfur battery positive electrode material to the sulfur powder to the carbon black to the binder is 6:1:2: 1.
Further, the binder includes an oil-soluble binder or a water-soluble binder.
Further, the oil-soluble binder includes polyvinylidene fluoride; the water-soluble binder comprises any one of polytetrafluoroethylene, polyethylene oxide, LA133, polymethyl methacrylate, beta-cyclodextrin, agar, starch, sodium carboxymethyl cellulose, polybutadiene rubber and styrene butadiene rubber.
Further, the oil-soluble binder and the water-soluble binder need to be prepared into a solution for use; the solvent adopted for preparing the oil-soluble binder solution is N-methyl-2-pyrrolidone; the solvent used for preparing the water-soluble binder solution is water.
Still further, the current collector is a carbon-coated aluminum foil.
The invention discloses the following technical effects:
(1) the multi-transition metal sulfide contained in the composite material prepared by the invention has a plurality of active sites and can simultaneously enhance Li 2 S 8 、Li 2 S 6 、Li 2 S 4 And the oxidation-reduction reaction of polysulfide with different molecular structures. The multi-element transition metal sulfide can also enhance the electrocatalytic activity by lowering a potential barrier so as to accelerate the electrochemical conversion; and the graphene oxide has the advantages of high conductivity, good toughness, large specific surface area, good chemical inertness and the like. The characteristics of the multi-element transition metal sulfide and the graphene oxide are combined, so that the volume change of sulfur can be adapted, the high sulfur loading capacity is realized, the shuttle effect is inhibited, the cycle life is prolonged, and the lithium-sulfur battery can keep the charging and discharging stability.
(2) FeCoS prepared by adopting method 2 Under the current density of 0.5C, the initial discharge specific capacity of the lithium-sulfur battery positive plate prepared from the/rGO composite material is 1117 mAh.g -1 After 100 cycles of the circulation process, the specific discharge capacity is still 688mAh g -1 And the coulombic efficiency is always kept above 96%, and the composite material has high specific capacity and lengthCycle life and the like.
(3) FeCoS prepared by the invention 2 The graphene oxide in the/rGO composite material can be used as a conductive carrier of a sulfur anode to make up the defect of poor sulfur conductivity, namely FeCoS 2 Metal cation in (2) to S in discharge process 2- Has an attraction effect, can inhibit the combination of sulfur and lithium, thereby inhibiting the volume expansion of the electrode material, and improving the electrochemical performance and the cycle life of the material.
(4) The invention prepares FeCoS with a two-dimensional layered structure 2 the/rGO composite material has higher catalytic activity, excellent adsorption on polysulfide, higher electrochemical performance and good conductivity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is FeCoS prepared in example 1 of the present invention 2 XRD diffractogram of/rGO composite;
FIG. 2 is FeCoS prepared in example 1 of the present invention 2 Transmission electron microscopy of/rGO composite;
FIG. 3 is FeCoS prepared in example 1 of the present invention 2 A crystal structure diagram of the/rGO composite material under a transmission electron microscope image;
FIG. 4 shows FeS 2 Electrochemical impedance spectrograms of the/rGO positive plate and the lithium-sulfur battery positive plate prepared in the embodiment 4 of the invention;
FIG. 5 is FeS 2 Cycle performance profiles for the/rGO positive electrode sheets and the lithium sulfur battery positive electrode sheets prepared in example 4 of the present invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in that stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and materials in connection with which they pertain. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including but not limited to.
Example 1
A preparation method of a multi-transition metal lithium-sulfur battery positive electrode material comprises the following steps:
(1) weighing 100mg of Graphene Oxide (GO), adding into 80mL of ethylene glycol, and performing ultrasonic dispersion for 2h to obtain a graphene oxide dispersion liquid.
(2) 1mmol of FeCl 2 ·4H 2 O、1mmol CoCl 2 ·6H 2 And adding O and 2mmol of thiourea into the graphene oxide dispersion liquid, and stirring for 2 hours to dissolve to obtain a mixed solution.
(3) Transferring the mixed solution into a 100mL polytetrafluoroethylene lining high-pressure reaction kettle, carrying out hydrothermal reaction for 12h at 200 ℃, cooling, washing with absolute ethyl alcohol and deionized water for 5 times, and then carrying out vacuum freeze drying for 24h to obtain the multi-transition metal lithium sulfur battery positive electrode material (FeCoS) 2 the/rGO composite material) has an XRD diffraction pattern shown in figure 1 and transmission electron microscope patterns shown in figures 2-3.
As can be seen from FIG. 1, FeCoS prepared by the present example 2 /rGO composite material (FeCoS) 2 /rGO nano sheet) sulfide is FeCoS 2 In accordance with standard cards.
As can be seen from FIG. 2, FeCoS prepared in this example 2 FeCoS in/rGO composite material 2 Uniformly growing on the laminated graphene sheet.
As can be seen from FIG. 3, FeCoS prepared in this example 2 FeCoS in/rGO composite material 2 The crystal lattice spacing is 0.284nm for a single polycrystalline phase, and the (100) crystal plane is consistent with a standard card.
Example 2
A preparation method of a multi-transition metal lithium-sulfur battery positive electrode material comprises the following steps:
(1) weighing 50mg of Graphene Oxide (GO), adding into 80mL of ethylene glycol, and performing ultrasonic dispersion for 2 hours to obtain a graphene oxide dispersion liquid.
(2) 1mmol of FeCl 2 ·4H 2 O、1mmol CoCl 2 ·6H 2 And adding O and 2mmol of thiourea into the graphene oxide dispersion liquid, and stirring for 2 hours to dissolve to obtain a mixed solution.
(3) Transferring the mixed solution into a 100mL polytetrafluoroethylene lining high-pressure reaction kettle, carrying out hydrothermal reaction for 12h at 200 ℃, cooling, washing with absolute ethyl alcohol and deionized water for 5 times, and then carrying out vacuum freeze drying for 24h to obtain the multi-transition metal lithium sulfur battery positive electrode material (FeCoS) 2 a/rGO composite).
The difference between the embodiment 1 and the embodiment 2 is that the amount of the graphene oxide is different, the amount of the graphene oxide in the embodiment 1 is 100mg, the amount of the graphene oxide in the embodiment 2 is 50mg, and the amount of the graphene oxide is adjusted to 50mg (embodiment 2), so that the performance of the prepared composite material is equivalent to that of the embodiment 1; adjusting the amount of graphene from 100mg to 50mg had no significant effect on the performance of the multi-transition metal lithium sulfur battery positive electrode material.
Comparative example 1
Comparative cathode material FeS 2 The preparation method of/rGO comprises the following steps:
(1) weighing 100mg of Graphene Oxide (GO), adding into 80mL of ethylene glycol, and performing ultrasonic dispersion for 2h to obtain a graphene oxide dispersion liquid.
(2) 1mmol of FeCl 2 ·4H 2 And adding O and 2mmol of thiourea into the graphene oxide dispersion liquid, and stirring for 2 hours to dissolve to obtain a mixed solution.
(3) Transferring the mixed solution into a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 12h at 200 ℃, cooling, washing with absolute ethyl alcohol and deionized water for 5 times, and carrying out vacuum freeze drying for 24h to obtain a comparative cathode material (FeS) 2 /rGO composite material)
Example 3
A preparation method of a lithium-sulfur battery positive plate comprises the following steps:
(1) sublimed sulfur powder and FeCoS prepared in example 1 are weighed according to the mass ratio of 6:1:2:1 2 a/rGO composite, carbon black and a binder PVDF (polyvinylidene fluoride).
(2) FeCoS (FeCoS) 2 Mixing, stirring and grinding the/rGO composite material, the sublimed sulfur powder, the carbon black and the binder for 30min, adding a solvent NMP, and grinding for 10min to prepare slurry.
(3) And (3) uniformly coating the slurry on a current collector (carbon-coated aluminum foil) with the coating thickness of 250 mu m, and drying at 60 ℃ for 12h under a vacuum condition to obtain the lithium-sulfur battery positive plate.
With FeS 2 Positive plate (FeS) prepared from/rGO composite material 2 /rGO positive plate) as control, FeS was added 2 Button batteries are assembled by the aid of the/rGO positive plate and the lithium-sulfur battery positive plate prepared by the method. Determination of FeS 2 rGO positive plate and lithium-sulfur battery positive electrode prepared by using sameThe resistance of the sheet, and the results are shown in fig. 4, where the abscissa Z' in fig. 4 is the real part of the impedance and the ordinate Z ″ is the imaginary part (negative) of the impedance.
As can be seen from FIG. 4, FeCoS prepared by the method of example 1 of the present invention 2 Resistance ratio FeS of lithium-sulfur battery positive plate prepared from/rGO composite material 2 the/rGO positive plate has small resistance and electrochemical performance advantages.
Determination of FeS 2 The cycling performance of the/rGO positive electrode sheet and the lithium sulfur battery positive electrode sheet at a current density of 0.5C is shown in fig. 5.
As can be seen from FIG. 5, the initial specific discharge capacity of the positive plate of the lithium-sulfur battery prepared according to the present invention was 1117mAh · g at a current density of 0.5C -1 After 100 cycles, the specific discharge capacity is still 688mAh g -1 And the coulombic efficiency is always kept above 96%, and the stable cycle life is realized. With FeS 2 Compared with the rGO positive plate, the positive plate of the lithium-sulfur battery contains the multi-element transition metal sulfide (FeCoS) 2 ) Has multiple active sites and enhances Li 2 S 8 、Li 2 S 6 、Li 2 S 4 And the multi-element transition metal compound can also enhance the electrocatalytic activity by lowering potential barrier so as to accelerate the electrochemical conversion.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (10)

1. A preparation method of a multi-transition metal lithium-sulfur battery positive electrode material is characterized by comprising the following steps: adding two transition metal salts and thiourea into the graphene oxide dispersion liquid, uniformly stirring, and carrying out hydrothermal reaction to obtain the multi-transition metal lithium-sulfur battery positive electrode material.
2. The method for preparing the multi-transition metal lithium sulfur battery positive electrode material according to claim 1, wherein the preparation of the graphene oxide dispersion specifically comprises: adding graphene oxide into ethylene glycol, and performing ultrasonic dispersion for 1-3 hours to obtain the graphene oxide dispersion liquid.
3. The method for preparing a multi-transition metal lithium sulfur battery positive electrode material according to claim 1, wherein the transition metal salt comprises an iron salt and a cobalt salt; the molar ratio of the ferric salt to the cobalt salt to the thiourea is 1:1: 2; the stirring time is 1-2 h; the temperature of the hydrothermal reaction is 200 ℃ and the time is 12 h.
4. A multi-transition metal lithium-sulfur battery cathode material prepared by the preparation method of any one of claims 1 to 3.
5. Use of the multiple transition metal lithium sulfur battery positive electrode material of claim 4 in the preparation of a lithium sulfur battery.
6. The positive plate of the lithium-sulfur battery is characterized in that a raw material comprises a current collector and a coating layer coated on the surface of the current collector; the coating layer includes the multi-transition metal lithium sulfur battery positive electrode material of claim 4.
7. The method for preparing the positive plate of the lithium-sulfur battery as claimed in claim 6, characterized by comprising the following steps:
and mixing and stirring the multi-element transition metal lithium-sulfur battery positive electrode material, sulfur powder, carbon black and a binder to prepare slurry, uniformly coating the slurry on a current collector, and drying to obtain the lithium-sulfur battery positive electrode plate.
8. The method for preparing the positive plate of the lithium-sulfur battery according to claim 7, wherein the mass ratio of the sulfur powder, the multi-transition metal lithium-sulfur battery positive electrode material, the carbon black and the binder is 6:1:2: 1.
9. The method for preparing a positive electrode sheet for a lithium-sulfur battery according to claim 7, wherein the binder comprises an oil-soluble binder or a water-soluble binder.
10. The method for preparing a positive electrode sheet for a lithium-sulfur battery according to claim 9, wherein the oil-soluble binder comprises polyvinylidene fluoride; the water-soluble binder comprises any one of polytetrafluoroethylene, polyethylene oxide, LA133, polymethyl methacrylate, beta-cyclodextrin, agar, starch, sodium carboxymethyl cellulose, polybutadiene rubber and styrene butadiene rubber.
CN202210977790.3A 2022-08-16 2022-08-16 Multi-transition metal lithium-sulfur battery positive electrode material and preparation method and application thereof Pending CN115057480A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109742359A (en) * 2019-01-07 2019-05-10 清华大学深圳研究生院 Lithium sulfur battery anode material, preparation method, positive plate and lithium-sulfur cell

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109742359A (en) * 2019-01-07 2019-05-10 清华大学深圳研究生院 Lithium sulfur battery anode material, preparation method, positive plate and lithium-sulfur cell

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* Cited by examiner, † Cited by third party
Title
X. CHEN ET AL.: ""Flower-like spherical FeCoS2 coated by reduced graphene oxide as anode for high performance potassium ion storage"", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *

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