CN110048102B - TiS2Preparation method of @ graphene composite nano material and application of material in lithium ion battery - Google Patents

TiS2Preparation method of @ graphene composite nano material and application of material in lithium ion battery Download PDF

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CN110048102B
CN110048102B CN201910292425.7A CN201910292425A CN110048102B CN 110048102 B CN110048102 B CN 110048102B CN 201910292425 A CN201910292425 A CN 201910292425A CN 110048102 B CN110048102 B CN 110048102B
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graphene
lithium ion
ion battery
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composite nano
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CN110048102A (en
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田小东
吕显国
褶春波
张耀
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Xinwangda Power Technology Co ltd
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Sunwoda Electric Vehicle Battery Co Ltd
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    • 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
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a TiS2A preparation method of a @ graphene composite nano material and application of the material in a lithium ion battery, belonging to the technical field of lithium ion battery materials. The preparation method comprises the following steps: ultrasonically dispersing graphite oxide in octadecylene to obtain a graphene oxide turbid liquid; uniformly stirring titanium source, sulfur source, oleic acid, octadecylene and graphene oxide suspension, heating to 260-320 ℃, reacting for 0.5-3h in inert atmosphere, centrifugally separating and drying reactants to obtain TiS2@ graphene composite nanomaterial. When the material obtained by the invention is used as a lithium ion battery cathode material, the material has higher specific capacity and better cycle performance.

Description

TiS2Preparation method of @ graphene composite nano material and application of material in lithium ion battery
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to TiS2The @ graphene composite nano material, the preparation method thereof and the application thereof in the lithium ion battery.
Background
With the rapid development of portable electronic devices, the increasing demand of pure electric or hybrid electric vehicles, and the requirement of renewable energy technology for power grid-scale energy storage, people are urgently required to develop rechargeable energy storage technology with high energy density, high power density and long-life cycle. Rechargeable lithium ion batteries have received great attention as one of green energy sources. Most of lithium ion battery negative electrode materials used commercially at present are graphite materials, the theoretical capacity of the graphite materials is only 372 mAh/g, and the development of graphite commercialization is greatly limited.
Transition metal disulfides are considered promising negative electrode materials for lithium batteries because of their unique layered structure, high theoretical specific capacity, and high conductivity. Among the different transition metal dichalcogenides, TiS2The lithium ion battery has the characteristics of light weight, low price, high lithium ion diffusion rate, small volume change in the discharging/charging process and the like. However, TiS2Irreversible changes to the electrode, such as surface passivation, chemical structure deformation, and formation of lithium dendrites, can occur, which can seriously affect the performance of the battery. One solution to this is to use TiS2In which carbon material is introduced, on the one hand, mayThe conductivity of the composite is improved, and the carbon material can buffer the volume change caused by lithium intercalation. It has been shown that doping CNTs to TiS2And the initial capacity is 450mAh/g, and can be maintained at 80% after 50 cycles. However, this method only combines CNTs and TiS2Simple physical mixing is performed, and a functionalized structure is not formed, so that the improvement effect is limited.
The invention successfully synthesizes TiS by a simple solvothermal method2@ graphene composite nanomaterial. TiS when used as a negative electrode material for lithium ion batteries2The @ graphene nano material has excellent cycling stability, and after 200 circles of cycling at a current density of 200mA/g, the material can keep a reversible capacity of 728 mAh/g. The invention has great significance for developing a method for functional nanometer materials.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention mainly aims to provide a TiS2A preparation method of a @ graphene composite nano material.
Another object of the present invention is to provide a TiS prepared by the above method2@ graphene composite nanomaterial.
It is still another object of the present invention to provide the above TiS2The application of the @ graphene composite nano material as a high-performance lithium ion battery negative electrode material.
The purpose of the invention is realized by the following technical scheme.
TiS2The preparation method of the @ graphene composite nanomaterial is solvothermal, and specifically comprises the following steps:
(1) ultrasonically dispersing graphite oxide in octadecylene to obtain a graphene oxide turbid liquid;
(2) charging TiCl into the reaction vessel4Uniformly stirring oleic acid, octadecene and the graphene oxide turbid liquid in the step (1) for 10 min;
(3) adding Na into the reaction vessel2S, wherein the mass ratio of the titanium source to the sulfur source is 1:1-1:10, pumping out gas by using a mechanical pump, introducing protective gas, and then heatingAt 260 ℃ and 320 ℃, the condensation reflux is maintained for 0.5 to 3 hours. After the reaction is finished, cooling to room temperature, washing by using a mixed solvent of cyclohexane and ethanol (1: 1), and then carrying out centrifugal separation to obtain a precipitate, wherein the precipitate is TiS2@ graphene composites.
Further, the introduced protective gas is inert gas, such as nitrogen and argon;
further, the graphite oxide is graphene oxide synthesized by using a Hummers method;
further, the TiS2The mass fraction of graphene in the composite nanomaterial of @ graphene is 5% -60%; (ii) a
In the above preparation method, Na2And S is used as a reducing agent to reduce the graphene oxide into graphene.
A TiS as described above2The application of the composite nano material of @ graphene as a lithium ion battery negative electrode material.
Preferably, the above specific application process is: mixing TiS2And mixing the composite nano material of the @ graphene, the carbon black and the PVDF according to the ratio of 8:1:1 to prepare pulp, and then coating the pulp on a copper foil to obtain the lithium ion battery cathode.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention adopts simple solvent heat to synthesize TiS2The composite nano material of the @ graphene is successfully applied to the negative electrode material of the lithium ion battery. TiS2The nano particles are anchored on the surface of the graphene, so that the volume change of the compound in the charge and discharge process is effectively relieved, and TiS is inhibited2The agglomeration of the nano particles increases the conductivity and improves the electrochemical stability of the material.
(2) The invention utilizes NaS2And reducing the graphene oxide. Compared with hydrazine reduction, the method does not introduce nitrogen element into the graphene, so that the obtained graphene has good conductivity and high purity; with NaBH4Compared with the prior art, the method has high reduction efficiency; compared with NaOH and vitamin C, the method has a large reduction degree.
(3) According to the invention, octadecylene is added as a solvent, oleic acid is used as a surfactant, and the obtained particles are uniformly dispersed and do not agglomerate.
(4) TiS in the present invention2In the composite nanomaterial of @ graphene, TiS2Anchored to graphene, thus TiS during cycling2The particles do not agglomerate.
(5) TiS of the invention2The composite nanomaterial of @ graphene has good cycle performance when used for a lithium ion battery cathode: when the mass fraction of graphene is 13.6-58.7%, the current density of the composite nano material is 200mA g-1After the circulation is performed for 200 circles, the reversible capacity is 520-728 mAh g-1. Therefore, the lithium ion negative electrode material prepared by the invention has better cycle performance.
Drawings
FIG. 1 shows TiS obtained according to the invention in example 22TEM images of composite nanomaterials of @ graphene.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Comparative example
(1) 4mmol of TiCl are introduced into the reaction vessel48mL of oleic acid and 35mL of octadecene, and uniformly stirring for 10 min;
(2) 5mmol of Na are added to the reaction volume2And S, pumping out gas by using a mechanical pump, introducing protective gas, heating to 280 ℃, and maintaining condensation reflux for 2 hours. After the reaction is finished, cooling to room temperature, washing by using a mixed solvent of cyclohexane and ethanol (1: 1), and then carrying out centrifugal separation to obtain a precipitate, wherein the precipitate is TiS2And (3) nano materials. 0.2g of TiS prepared in this example was weighed2Mixing and grinding the nano material, 0.025 g of PVDF and 0.025 g of carbon black, transferring the mixture into a small glass bottle, adding 1 ml of NMP, magnetically stirring for 4 hours, coating the material on copper foil to prepare an electrode, assembling the electrode in a glove box by using metal lithium as a counter electrode to form the CR2016 type button battery, and testing the electrochemical performance.
Example 1
(1) Ultrasonically dispersing 0.2g of graphite oxide in 20mL of octadecene to obtain a graphene oxide turbid liquid;
(2) 10mmol TiCl are introduced into the reaction vessel48mL of oleic acid, 15mL of octadecene and the liquid in the step (1) are uniformly stirred for 10 min;
(3) adding 10mmol of Na into the reaction volume2And S, pumping out gas by using a mechanical pump, introducing protective gas, heating to 240 ℃, and maintaining condensation reflux for 0.5 h. After the reaction is finished, cooling to room temperature, washing by using a mixed solvent of cyclohexane and ethanol (1: 1), and then carrying out centrifugal separation to obtain a precipitate, wherein the precipitate is TiS2@ graphene composites. 0.2g of TiS prepared in this example was weighed2The composite material of @ graphene, 0.025 g PVDF and 0.025 g carbon black are mixed and ground, then transferred into a small glass bottle, 1 ml of NMP is added, magnetic stirring is carried out for 4 hours, the material is coated on copper foil to prepare an electrode, metal lithium is used as a counter electrode to be assembled into a CR2016 type button cell in a glove box, and electrochemical performance test is carried out.
Example 2
(1) Ultrasonically dispersing 0.2g of graphite oxide in 20mL of octadecene to obtain a graphene oxide turbid liquid;
(2) 4mmol of TiCl are introduced into the reaction vessel48mL of oleic acid, 15mL of octadecene and the liquid in the step (1) are uniformly stirred for 10 min;
(3) 5mmol of Na are added to the reaction volume2And S, pumping out gas by using a mechanical pump, introducing protective gas, heating to 280 ℃, and maintaining condensation reflux for 2 hours. After the reaction is finished, cooling to room temperature, washing by using a mixed solvent of cyclohexane and ethanol (1: 1), and then carrying out centrifugal separation to obtain a precipitate, wherein the precipitate is TiS2The nanomaterial, a TEM image thereof is shown in fig. 1. 0.2g of TiS prepared in this example was weighed2Mixing and grinding the nano material, 0.025 g of PVDF and 0.025 g of carbon black, transferring the mixture into a small glass bottle, adding 1 ml of NMP, magnetically stirring for 4 hours, coating the material on copper foil to prepare an electrode, assembling the electrode in a glove box by using metal lithium as a counter electrode to form the CR2016 type button battery, and testing the electrochemical performance.
Example 3
(1) Ultrasonically dispersing 0.2g of graphite oxide in 20mL of octadecene to obtain a graphene oxide turbid liquid;
(2) 3mmol TiCl are added to the reaction vessel48mL of oleic acid, 15mL of octadecene and the liquid in the step (1) are uniformly stirred for 10 min;
(3) 15mmol of Na are added to the reaction volume2And S, pumping out gas by using a mechanical pump, introducing protective gas, heating to 300 ℃, and maintaining condensation reflux for 2 hours. After the reaction is finished, cooling to room temperature, washing by using a mixed solvent of cyclohexane and ethanol (1: 1), and then carrying out centrifugal separation to obtain a precipitate, wherein the precipitate is TiS2@ graphene composites. 0.2g of TiS prepared in this example was weighed2The composite material of @ graphene, 0.025 g PVDF and 0.025 g carbon black are mixed and ground, then transferred into a small glass bottle, 1 ml of NMP is added, magnetic stirring is carried out for 4 hours, the material is coated on copper foil to prepare an electrode, metal lithium is used as a counter electrode to be assembled into a CR2016 type button cell in a glove box, and electrochemical performance test is carried out.
Example 4
(1) Ultrasonically dispersing 0.2g of graphite oxide in 20mL of octadecene to obtain a graphene oxide turbid liquid;
(2) 1.5mmol TiCl are introduced into the reaction vessel48mL of oleic acid, 15mL of octadecene and the liquid in the step (1) are uniformly stirred for 10 min;
(3) 15mmol of Na are added to the reaction volume2And S, pumping out gas by using a mechanical pump, introducing protective gas, heating to 320 ℃, and maintaining condensation reflux for 3 hours. After the reaction is finished, cooling to room temperature, washing by using a mixed solvent of cyclohexane and ethanol (1: 1), and then carrying out centrifugal separation to obtain a precipitate, wherein the precipitate is TiS2@ graphene composites. 0.2g of TiS prepared in this example was weighed2@ 0.025 g of PVDF and 0.025 g of carbon black are mixed and ground, then the mixture is transferred into a small glass bottle, 1 ml of NMP is added, magnetic stirring is carried out for 4 hours, the material is coated on copper foil to prepare an electrode, metal lithium is adopted as a counter electrode to be assembled into a CR2016 type button cell in a glove box, and then the CR2016 type button cell is fed into the glove boxAnd (6) carrying out electrochemical performance test.
And (3) performance testing:
the material prepared in the above embodiment uses X-ray diffraction technology (XRD), Raman spectroscopy (Raman Spectra), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), and thermogravimetric analysis (TGA) as characterization means to analyze the composition, morphology, particle size, and graphite content thereof.
After the battery prepared in the embodiment is placed for 12 hours, a battery tester (Shenzhen Xinwei) is adopted, the testing temperature is room temperature, and the current density is 200mA g-1~1000mA g-1In the case of (2), the battery was subjected to constant current charge and discharge (discharge cutoff voltage of 0.01V, charge voltage of 3V), and the cycle performance and rate performance of the battery were tested. The electrical properties of the samples are detailed in table 1.
TABLE 1
Figure DEST_PATH_IMAGE001
Note: in the table, "content of graphene" means the mass fraction of graphite in the product, obtained by a thermal analyzer.
The invention prepares TiS by utilizing a hot solvent method2The composite nano material of @ graphene is characterized in that the synthesis conditions of the material are researched through the reaction temperature, the reaction time and the proportion of titanium and sulfur, and the electrochemical performance of the corresponding material when the material is used for a lithium ion battery cathode is researched. By comparing 5 examples, it was found that a sample with a titanium to sulfur ratio of 4:5 and a graphite olefin mass fraction of 24.3% had good cycle performance and was able to operate at 200mA g-1After circulating 200 circles under the current density, 728mAh g is kept-1The above reversible capacity, even at a large current density (1000 mAg)-1) After 300 cycles, 346mAhg can be maintained-1The reversible capacity of (a).
The present invention is not limited to the above-described embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (6)

1. TiS2The preparation method of the @ graphene composite nanomaterial is characterized by comprising the following steps of:
(1) ultrasonically dispersing graphite oxide in octadecylene to obtain a graphene oxide turbid liquid;
(2) adding a titanium source, oleic acid, octadecene and the graphene oxide suspension liquid obtained in the step (1) into a reaction container, wherein the titanium source is TiCl4Stirring uniformly;
(3) then adding a sulfur source into the reaction vessel, wherein the mass ratio of the titanium source to the sulfur source is 1:1-1:10, and the sulfur source is Na2S, pumping out gas by using a mechanical pump, introducing protective gas, heating to 260-320 ℃, maintaining condensation reflux for 0.5-3h, adding an organic solvent for washing after the reaction is finished, and performing centrifugal separation and drying to obtain TiS2@ graphene composite nanomaterial.
2. The method according to claim 1, wherein the graphite oxide is graphite oxide synthesized by Hummers method.
3. The method of claim 1, wherein the TiS is produced by2Anchored to the graphene.
4. The method according to claim 1, wherein the graphene oxide is obtained by passing Na2And S is reduced into graphene.
5. The method of claim 1, wherein the TiS is produced by2The mass fraction of graphene in the composite nanomaterial of @ graphene is 5-60%.
6. TiS produced by the production method according to any one of claims 1 to 52Composite nano material of @ grapheneThe application of the lithium ion battery cathode material is characterized in that the specific application process is as follows: mixing TiS2And mixing the composite nano material of the @ graphene, carbon black and PVDF to prepare pulp, and coating the pulp on copper foil to obtain the lithium ion battery cathode.
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