CN113964315A - Preparation method and application of large-size two-dimensional lithium titanate nanosheet - Google Patents
Preparation method and application of large-size two-dimensional lithium titanate nanosheet Download PDFInfo
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- CN113964315A CN113964315A CN202111206743.0A CN202111206743A CN113964315A CN 113964315 A CN113964315 A CN 113964315A CN 202111206743 A CN202111206743 A CN 202111206743A CN 113964315 A CN113964315 A CN 113964315A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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
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- Y02E60/10—Energy storage using batteries
Abstract
The embodiment of the invention discloses large-size two-dimensional lithium titanate (Li)4Ti5O12) Nanosheets, and a preparation method and application thereof. The two-dimensional lithium titanate nanosheet is formed by assembling lithium titanate nanoparticles on the surface of graphene, has a hierarchical pore structure, a sample with a reserved graphene substrate is a graphene-based two-dimensional lithium titanate nanosheet, a sample doped with other elements is the graphene-based element-doped two-dimensional lithium titanate nanosheet, and the sample without the graphene substrate is the pure two-dimensional lithium titanate nanosheet. The graphene-based lithium titanate nanosheet is graphene-based amorphous TiO2The film is a precursor, in N2The lithium titanate is generated by high-temperature reaction with LiOH under protection, the multi-level pore structure and the high specific surface area of the lithium titanate are favorable for the adsorption and transfer of lithium ions, the conductivity of the lithium titanate can be improved after the elements are doped,meanwhile, the graphene is used as a conductive substrate, so that the conductivity of the composite material can be improved. The two-dimensional lithium titanate nanosheet can be used as a negative electrode material of a lithium ion battery, shows excellent electrochemical performance and has pseudocapacitance behavior.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a large-size two-dimensional lithium titanate nanosheet, and a preparation method and application thereof.
Background
Lithium Ion Batteries (LIBs) are widely used in Electric Vehicles (EVs), portable electronic products and power grid energy storage systems due to their advantages of low cost, high energy density, long cycle life, and environmental friendliness. The graphite has the advantages of high stability, good conductivity and abundant resources, and the theoretical specific capacity is 372mA h g-1Therefore, the lithium ion battery anode material is used as a lithium ion battery anode material and is commercialized. However, Li+The potential of the intercalated graphite is close to that of lithium metal (0-0.25V vs. Li)+/Li), lithium dendrites can form when the battery is overcharged, creating a safety hazard. At the same time, the electrolyte reacts with graphite at this voltage to form a thick and unstable Solid Electrolyte Interphase (SEI) layer, resulting in low initial coulombic efficiency, specific capacity decay, and an increase in resistance. In view of the problems of low initial coulombic efficiency, poor rate capability and the like, commercial graphite cannot meet the increasing energy demand.
Spinel Li4Ti5O12(LTO) is considered the most promising negative electrode material for lithium ion batteries because of its high rate and long lifetime. LTO has almost no change in volume during the lithium intercalation/deintercalation process (<0.2%) and is therefore referred to as a "zero strain" intercalation material. In addition, LTO has a high lithium insertion potential (1.55V vs. Li)+/Li), the formation of SEI films and lithium dendrites can be avoided, thereby ensuring the safety of LIBs. However, as a lithium ion battery anode material, LTO still has some problems. Although LTO exhibits better cycling stability and structural stability than graphite at high rates, its theoretical specific capacity is lower than that of graphite, only 175mA h g-1. Another disadvantage of LTO is electron conductivity and Li+Coefficient of diffusion (D)Li) Worse, this problem greatly reduces the rate capability of LTO.
Disclosure of Invention
The embodiment of the invention discloses a large-size two-dimensional lithium titanate nanosheet, a preparation method and application thereof, wherein the large-size two-dimensional lithium titanate nanosheet is used as a negative electrode active substance of a lithium ion battery and can improve the performance of the lithium ion battery.
The invention firstly provides a lithium ion battery cathode material which is composed of graphene and lithium titanate nanosheets positioned on the surfaces of the graphene, wherein the lithium titanate nanosheets are formed by assembling lithium titanate nanoparticles and have a special hierarchical pore structure.
The invention also provides a preparation method of the two-dimensional lithium titanate nanosheet, which comprises the following steps:
preparing graphene oxide by a hummer method, adding the graphene oxide and tetrabutyl titanate into 60mL of cyclohexane, stirring for two weeks, centrifuging, adding the obtained solid into 80mL of cyclohexane, reacting for 6 hours under a hydrothermal condition, centrifuging, washing and drying to obtain a graphene-based amorphous titanium dioxide film;
adding the graphene-based titanium dioxide film into a lithium hydroxide solution, stirring for 12 hours, drying in an oven to remove a solvent, transferring the obtained solid into a tubular furnace, heating at 700-900 ℃ for 5-10 hours under the protection of nitrogen, and cooling to room temperature to obtain the graphene-based lithium titanate nanosheet.
The embodiment of the invention also discloses a lithium ion battery cathode which takes the cathode material as a cathode active material.
In a preferred embodiment of the present invention, the template for synthesizing lithium titanate is selected from graphene.
In a preferred embodiment of the present invention, the lithium source of the synthetic lithium titanate is lithium hydroxide.
In a preferred embodiment of the present invention, the kind of inorganic salt used is chromium nitrate.
The embodiment of the invention also discloses a lithium ion battery which comprises the lithium ion battery cathode.
In a preferred embodiment of the invention, the lithium ion battery is in the form of a 2032 button cell.
According to the technical scheme, amorphous TiO is formed by controllable hydrolysis of tetrabutyl titanate on the surface of graphene oxide2And the nano film is reacted with LiOH at high temperature to generate a large-size two-dimensional nano sheet assembled by LTO nano particles of 6-10 nm. The material has larger pores formed by stacking LTO nano-particles and TiO2A multi-stage pore canal structure formed by micro mesopores (1.3-1.6 nm/2.7-3.4 nm) remained on the nanometer film precursor. The hierarchical pores not only promote Li+Diffused and is Li+Provides a larger interface. Meanwhile, the electronic conductivity of the LTO composite material can be improved by using the graphene substrate as a conductive carrier, so that the material has better electrochemical performance。
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is an X-ray diffraction pattern of graphene-based lithium titanate nanoplates prepared in example 1;
fig. 2 is a projection electron microscope image of graphene-based lithium titanate nanoplates prepared in example 1;
fig. 3 is a long cycle performance diagram of graphene-based lithium titanate nanoplates prepared in example 1;
fig. 4 is a cyclic voltammetry graph of graphene-based lithium titanate nanoplates prepared in example 1.
Detailed Description
Formation of amorphous TiO by controlled hydrolysis of tetrabutyl titanate on graphene oxide surfaces2And the nano film is reacted with LiOH at high temperature to generate a large-size two-dimensional nano sheet assembled by LTO nano particles of 6-10 nm. The material has a hierarchical pore structure. The invention also provides a lithium ion battery cathode using the battery cathode material as a cathode active material. The template for synthesizing the material comprises but is not limited to graphene, MXene and carbon cloth, and graphene is preferred. Meanwhile, the lithium source for synthesizing the material comprises lithium carbonate, lithium hydroxide and lithium acetate, and preferably lithium hydroxide. The lithium ion battery cathode provided by the invention can be in a sheet shape or other shapes, and when the lithium ion battery cathode is in the sheet shape, the lithium ion battery cathode can be called as a lithium ion battery cathode sheet. The lithium ion battery provided by the invention can be obtained by assembling the lithium ion battery cathode provided by the invention with the anode, the diaphragm, the electrolyte and the like; it should be noted that, when the lithium ion battery provided by the present invention is assembled, the adopted positive electrode, separator, electrolyte solution, etc. can all adopt materials commonly used in the prior art for assembling lithium ion batteries, and the present invention does not need to be further described hereinAnd (4) defining a row. Similarly, the method for assembling the lithium ion battery is also the prior art, and the invention is not limited herein. The lithium ion battery provided by the invention can be a 2032 button cell battery and the like.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
First, a method for producing graphene oxide will be described. The graphene oxide adopted in the invention can be prepared by an improved Hummer method, and the specific flow comprises the following steps: natural flake graphite (5g), concentrated sulfuric acid (230mL, 98%) and sodium nitrate (NaNO)35g) are mixed, cooled under ice bath condition without stopping stirring by a glass rod, and after uniform mixing, potassium permanganate (KMnO) is slowly added430g) to control the temperature of the reaction system. Then the reaction vessel is placed in a constant temperature water bath at about 35 ℃, stirred for 30min, added with deionized water (460mL) and subjected to oil bath, and the temperature of the reaction solution is controlled at about 98 ℃. Stirring for 15min, adding large amount of deionized water (1.4L) for washing, and adding hydrogen peroxide (30% H)2O225mL) at which time the solution changed from a brownish black color to a bright yellow color. After standing and aging, the mixture was filtered and washed with dilute hydrochloric acid (1: 10 vol., 2L). Fully washing with deionized water until no SO is contained in the filtrate4 2-(BaCl2Solution detection). Air drying at 65 deg.C, and storing under sealed condition.
Example 1
0.1g GO (graphene oxide) was dispersed in 30mL cyclohexane, and 3mL tetrabutyl titanate (C) was added16H36O4Ti), stirring for 2 weeks until GO is uniformly dispersed. Subsequently, the dispersion was centrifuged (10000r/min), the supernatant was decanted, the centrifuged solid was washed with cyclohexane 3 times, and the washed solid was redispersed in 40mL of cyclohexane and then transferredTransferring the mixture into a 100mL reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 6 hours, cooling to room temperature, centrifuging (10000r/min), pouring out the upper layer liquid, and drying at 40 ℃. The resulting material was then mixed with 20mL of 0.1M lithium hydroxide solution, stirred at 80 ℃ for 12h, and dried at 60 ℃. And finally, calcining for 10 hours (10 ℃/min at 700 ℃) in a high-temperature tubular furnace under the protection of nitrogen to obtain the lithium ion battery cathode material, namely the graphene-based lithium titanate.
Example 2
0.1g GO (graphene oxide) was dispersed in 30mL cyclohexane, and 3mL tetrabutyl titanate (C) was added16H36O4Ti), stirring for 2 weeks until GO is uniformly dispersed. Then the dispersion liquid is centrifuged (10000r/min), supernatant liquid is poured off, the solid obtained by centrifugation is washed by cyclohexane for 3 times, then the washed solid is dispersed in 40mL cyclohexane again, and then the solid is transferred to a 100mL reaction kettle, hydrothermal is carried out for 6 hours at 180 ℃, the solid is cooled to room temperature and then centrifuged (10000r/min), and the supernatant liquid is poured off and dried at 40 ℃. The resulting material was then mixed with chromium nitrate and 20mL of a 0.1M lithium hydroxide solution, stirred at 80 ℃ for 12 hours, and then dried at 60 ℃. And finally, calcining for 10 hours (10 ℃/min at 700 ℃) in a high-temperature tubular furnace under the protection of nitrogen to obtain the lithium ion battery cathode material, namely the chromium-doped graphene-based lithium titanate.
Example 3
0.1g GO (graphene oxide) was dispersed in 30mL cyclohexane, and 3mL tetrabutyl titanate (C) was added16H36O4Ti), stirring for 2 weeks until GO is uniformly dispersed. Then the dispersion liquid is centrifuged (10000r/min), supernatant liquid is poured off, the solid obtained by centrifugation is washed by cyclohexane for 3 times, then the washed solid is dispersed in 40mL cyclohexane again, and then the solid is transferred to a 100mL reaction kettle, hydrothermal is carried out for 6 hours at 180 ℃, the solid is cooled to room temperature and then centrifuged (10000r/min), and the supernatant liquid is poured off and dried at 40 ℃. The resulting material was then mixed with 20mL of 0.1M lithium hydroxide solution, stirred at 80 ℃ for 12h, and dried at 60 ℃. And finally calcining for 10 hours (10 ℃/min at 700 ℃) in a high-temperature tube furnace under the protection of nitrogen. The sample is subsequently calcined in a muffle furnace for 3h (500 ℃ C. 10 ℃ C.)min), and obtaining the lithium ion battery cathode material which is called lithium titanate nanosheet.
Sample characterization
1. X-ray diffraction (XRD) analysis
The graphene-based lithium titanate prepared in example 1 of the present invention was subjected to X-ray diffraction analysis using an X-ray powder diffractometer (model: X Pert PRO MPD) manufactured by parnacco, netherlands, and the analysis result is shown in fig. 1. As can be seen from the comparison between the XRD pattern of graphene-based lithium titanate in fig. 1 and the standard card of LTO, the diffraction peak of graphene-based lithium titanate is very fitted to the standard peak of LTO in the standard PDF card, which proves that the lithium titanate nanosheet is successfully obtained.
2. Transmission Electron Microscope (TEM) analysis
Scanning analysis of the graphene-based lithium titanate prepared in example 1 by using a transmission electron microscope (FEI Talos F200S) shows that, as shown in fig. 2, lithium titanate nanosheets formed by particle accumulation are clearly seen in fig. 2, and the particle size of LTO is about 6-10 nm.
Performance testing
Preparing a lithium ion battery negative plate: 0.6730g of polyvinylidene fluoride (PVDF) is dissolved in 10.5437g of N-methyl pyrrolidone (NMP) to form a solution with the mass fraction of 6%; the negative electrode material of the graphene-based lithium titanate battery prepared in example 1, PVDF and acetylene black (conductive agent) in the solution are mixed according to a mass ratio of 70:10:20, and the mixture is fully and uniformly ground. Transferring the ground sticky mixed slurry to a copper foil (negative current collector) cleaned by alcohol, then adjusting the height of a scraper of an automatic coating machine to be 15 micrometers, automatically coating the slurry on the surface of the copper foil, transferring the copper foil to a vacuum drying oven, and standing the copper foil for 12 hours at 80 ℃. And then separating the laid battery film from the glass by using tweezers, cutting the battery film into a circular negative plate with the diameter of 14 mm by using a film cutting machine, weighing the mass, and placing the negative plate in a glove box for later use.
Assembling 2032 button cell: the cell assembly was performed in a glove box filled with high purity argon. The specific process is as follows: placing lithium plate into negative electrode shell, laying diaphragm (PE film), adding 100 μ L electrolyte (solute of electrolyte is LiPF)6The solvent is formed by mixing ethylene carbonate/diethyl carbonate/dimethyl carbonate (EC/DEC/DMC) with the volume ratio of 1:1:1, and LiPF6The molar concentration of (1 mol/L). And after the electrolyte uniformly wets the diaphragm, adding the lithium ion battery negative plate prepared in the embodiment 1, then adding the steel plate and the elastic sheet, finally buckling the positive shell, filling the positive shell into a self-sealing bag, and sealing the bag. After removal from the glove box, the cells were immediately sealed on a sealer and allowed to stand for 12 hours. This battery is referred to as battery No. 1.
Comparative example 1
Preparing a battery cathode sheet by using chromium-doped graphene-based lithium titanate. The preparation process of comparative example 1 differs from that of battery No. 1 only in that the graphene-based lithium titanate material obtained in example 1 in battery No. 1 is replaced with the chromium-doped graphene-based lithium titanate material obtained in example 2, and the other preparation processes are the same as those of battery No. 1. This electrode is referred to as battery No. 2.
Comparative example 2
And preparing the battery negative plate by using the lithium titanate nano plate. The preparation process of comparative example 2 differs from that of battery No. 1 only in that the graphene-based lithium titanate material obtained in example 1 in battery No. 1 is replaced with the lithium titanate nanosheet material obtained in example 3, and the other steps are the same as those of battery No. 1. This electrode is referred to as a No. 3 cell.
The test results of the test on the LAND battery test system for the No. 1 battery, the No. 2 battery and the No. 3 battery are shown in fig. 3, and the test was performed under constant current, with the current density of 10C (1C: 175mA/g) and the voltage range of 1-2.5V. The test result is shown in fig. 3, and it can be seen that the capacity of the graphene-based lithium titanate can be still maintained at 168mA h g after 1000 cycles-1. The addition of the graphene can effectively improve the conductivity of the lithium titanate.
According to the formula i (V) ═ k1v+k2v1/2The pseudocapacitance contribution of cell number 1 was calculated. As shown in FIG. 4, it can be found that the cell number 1 has a charge of 10mV s-1At the sweep rate of (2), the contribution of pseudocapacitance is a little 76%. The multi-level pore structure and the larger specific surface area can provide pseudo capacitance, thereby increasing the capacity of the battery.
Through the tests, the performance of the battery manufactured by using the lithium ion battery cathode provided by the invention is greatly improved compared with that of commercial lithium titanate, and the actual capacity of the battery manufactured by using the lithium ion battery cathode provided by the invention exceeds the theoretical specific capacity, which shows that the material can provide extra capacity contribution (pseudo capacitance).
The lithium ion battery cathode material and the application thereof provided by the invention are described in detail above. The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its central concept. It should be noted that, for those skilled in the art, it is possible to make several improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the protection scope of the claims of the present invention.
Claims (10)
1. A large-size two-dimensional lithium titanate nanosheet is characterized by consisting of graphene and a lithium titanate nanosheet positioned on the surface of the graphene, wherein the lithium titanate nanosheet is formed by assembling lithium titanate nanoparticles, has a special hierarchical pore structure, and can be heated in air to remove the graphene so as to obtain a pure two-dimensional lithium titanate nanosheet;
the preparation method of the graphene-based lithium titanate nanosheet comprises the following steps:
preparing graphene oxide by a hummer method, adding the graphene oxide and tetrabutyl titanate into 60mL of cyclohexane, stirring for two weeks, centrifuging, adding the obtained solid into 80mL of cyclohexane, reacting for 6 hours under a hydrothermal condition, centrifuging, washing and drying to obtain a graphene-based amorphous titanium dioxide film;
adding the graphene-based titanium dioxide film into a lithium hydroxide solution, stirring for 12 hours, drying in an oven to remove a solvent, transferring the obtained solid into a tubular furnace, heating at 700-900 ℃ for 5-10 hours under the protection of nitrogen, and cooling to room temperature to obtain graphene-based lithium titanate nanosheets;
the preparation method of the graphene-based element doped lithium titanate nanosheet comprises the following steps:
adding a graphene-based titanium dioxide film and inorganic salts containing other elements into a lithium hydroxide solution, stirring for 12 hours, drying in an oven to remove a solvent, transferring the obtained solid into a tubular furnace, heating at 700-900 ℃ for 5-10 hours under the protection of nitrogen, and cooling to room temperature to obtain graphene-based element-doped lithium titanate nanosheets;
the preparation method of the pure lithium titanate nanosheet comprises the following steps:
transferring the prepared graphene-based lithium titanate nanosheets to a muffle furnace, heating the obtained graphene-based lithium titanate nanosheets in air at 500-900 ℃ for 2-5 hours, and removing graphene to obtain pure two-dimensional lithium titanate nanosheets;
or adding the graphene-based titanium dioxide film into a lithium hydroxide solution, stirring for 12 hours, drying in an oven to remove the solvent, transferring the obtained solid into a muffle furnace, and heating in the air at 600-900 ℃ for 2-5 hours to obtain pure two-dimensional lithium titanate nanosheets;
the mass ratio of the graphene oxide to tetrabutyl titanate is 1-5: 50;
the concentration of the lithium hydroxide solution is 0.1-0.2 mol/L;
the mass ratio of the graphene-based titanium dioxide to the lithium hydroxide solution is 1-8: 10;
the mass ratio of the graphene-based titanium dioxide to the inorganic salt containing other elements is 1-3: 1.
2. The method of claim 1, wherein the graphene substrate used can be replaced by MXene, black phosphorus, carbon cloth.
3. The process as claimed in claim 1, wherein the lithium hydroxide used is replaced by lithium nitrate, lithium carbonate or lithium acetate.
4. The lithium titanate nanoplate of claim 1, having a large-sized two-dimensional structure, a length and width of 1 to 5 μm, and a thickness of 20 to 100 nm.
5. The lithium titanate nanoplate of claim 1, which is composed of lithium titanate nanoparticles of 5 to 100nm, and the size of the particles can be controlled by the amount of reactants added, reaction atmosphere, reaction temperature and time.
6. The lithium titanate nanoplate of claim 1, having a hierarchical pore structure in which the pore diameter of the micropores is 0.5 to 2nm and the pore diameter of the mesopores is 2 to 50 nm.
7. The lithium titanate nanoplate of claim 1, having a specific surface area of 100 to 300m2Per g, the pore volume is 0.1-0.3 cm3/g。
8. The method of claim 1, wherein the inorganic salt species used include chlorides, sulfates, nitrates of iron, gallium, magnesium, aluminum, nickel, chromium, molybdenum, manganese, cobalt, vanadium, lanthanum, zirconium.
9. The graphene-based lithium titanate nanosheet, the graphene-based element-doped lithium titanate nanosheet and the pure lithium titanate nanosheet according to claim 1, wherein the graphene-based lithium titanate nanosheet, the pure lithium titanate nanosheet and the pure lithium titanate nanosheet are used as active materials of a positive electrode, and a 2032 button cell assembled by using a lithium sheet as a negative electrode can show obvious pseudocapacitance behavior in a performance test.
10. The graphene-based lithium titanate nanosheet, the graphene-based element-doped lithium titanate nanosheet, and the pure lithium titanate nanosheet of claim 1, all of which are useful as negative active materials for lithium ion batteries to enhance the performance of the lithium ion batteries.
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