CN109148858B - Lithium titanate-titanium dioxide composite material and preparation method and application thereof - Google Patents
Lithium titanate-titanium dioxide composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a lithium titanate-titanium dioxide composite material and a preparation method and application thereof, and belongs to the technical field of lithium batteries. According to the method, a lithium source and micron-sized titanium dioxide are mixed, then the mixture reacts at 160-200 ℃ for 10-20 hours, and the mixture is calcined in air at 700 ℃ for 2 hours after the reaction to obtain the lithium titanate-titanium dioxide composite material. The method of the invention can be used for preparing micron-sized TiO2Synthesis of Li4Ti5O12Material, and in TiO2Surface formation of nanoscale Li4Ti5O12Increasing the surface area of the material, and reducing the Li content of lithium ions and electrons4Ti5O12The transmission distance on the material and the doping generated at the two-phase interface of the lithium titanate-titanium dioxide composite material in the invention lead the prepared Li4Ti5O12The material can be mixed with nano-TiO2Synthetic Li4Ti5O12The material is comparable to the material.
Description
Technical Field
The invention relates to a lithium titanate-titanium dioxide composite material and a preparation method and application thereof, belonging to the technical field of lithium batteries.
Background
In recent years, environmental pollution and energy crisis gradually become two major challenges facing human sustainable development. With the proliferation of the population and the development of industrialization, the existing non-renewable resources have failed to meet the long-term development needs of the economy, and these traditional fossil energy sources cause serious environmental problems. Therefore, the development of renewable clean new energy has become a major problem to be solved by researchers.
The chemical power supply is a device capable of mutually converting and storing chemical energy and electric energy, plays an important role in reasonably utilizing various novel green energy sources, and has important practical significance for solving the problems of energy crisis and environmental pollution. Traditional chemical power sources comprise lead-acid batteries, nickel-cadmium batteries, nickel-oxygen batteries and the like, and the requirements of social sustainable development cannot be well met due to the defects of low energy density, serious environmental pollution, high self-discharge and the like.
Lithium ion batteries have been the focus of attention in various fields since the advent as novel energy storage devices. Compared with the traditional battery, the battery has the advantages of light weight, small volume, high energy density, long service life, no memory effect, no pollution and the like. In recent years, lithium ion batteries have already occupied a large share of the small-sized secondary battery market, and are widely used in various electronic products such as mobile phones, notebook computers, digital cameras, MP3, and the like.
Li4Ti5O12As a new lithium ion battery cathode material, the volume change before and after charging and discharging is only 0.3 percent due to a smaller volume effect, the material is called as a zero-strain material, and the cycle performance of the material is excellent. Furthermore, Li4Ti5012The charging and discharging voltage platform is long and stable, and the material can fully discharge under the condition of meeting the discharging voltage requirement. Li4Ti5O12Compared with carbon-based materials, the material has good cycle performance and good Li+The conductivity has the characteristics of more charging times, faster charging process and higher safety required by the next generation of lithium ion batteries, and the Li4Ti5O12Is an anode material with great application prospect.
At present stage, use TiO2Hydrothermal synthesis of Li4Ti5O12Mainly adopts nano-grade TiO2The purpose of which is to increase Li4Ti5O12The surface area of the material is reduced, and lithium ions and electrons are reduced in Li4Ti5O12Transport distance over materials, thereby increasing Li4Ti5O12Capacity and rate capability of the material. But nano-sized TiO2The price is higher, causes the lithium cell cost higher.
Disclosure of Invention
To solve the above problems, the present invention uses micron-sized TiO2Synthesis of Li4Ti5O12Material in TiO2Surface formation of nanoscale Li4Ti5O12Increasing the surface area of the material, and reducing the Li content of lithium ions and electrons4Ti5O12The transmission distance on the material and the doping generated at the two-phase interface of the lithium titanate-titanium dioxide composite material in the invention lead the prepared Li4Ti5O12The material can be mixed with nano-TiO2Synthetic Li4Ti5O12The material is comparable to the material.
The invention provides a preparation method of a lithium titanate-titanium dioxide composite material, which comprises the following steps:
(1) adding micron-sized titanium dioxide into 0.2-0.6M lithium hydroxide solution, and uniformly stirring to obtain a mixed solution;
(2) reacting the mixed solution obtained in the step (1) at 160-200 ℃ for 10-20 h to obtain a precursor;
(3) and (3) calcining the precursor prepared in the step (2) to obtain the lithium titanate-titanium dioxide composite material.
In one embodiment of the present invention, the micron-sized titanium dioxide has a particle size of 1 to 10 μm.
In one embodiment of the present invention, in the step (1), the molar ratio of lithium hydroxide to titanium dioxide is 1:1 to 1.5.
In one embodiment of the present invention, in the step (1), the stirring time is 2 to 10 hours.
In an embodiment of the present invention, the method further includes, after the precursor is obtained by the reaction in step (2), a step of washing and drying the precursor.
In one embodiment of the invention, the washing is carried out with water and ethanol, respectively.
In one embodiment of the present invention, the drying is performed at 60-80 ℃ for 3-5 h.
In one embodiment of the present invention, in the step (3), the calcination is performed at 600 to 800 ℃ for 2 to 4 hours.
The second purpose of the invention is to provide a lithium titanate-titanium dioxide composite material prepared by the method.
The second purpose of the invention is to provide a lithium battery negative electrode material prepared from the lithium titanate-titanium dioxide composite material prepared by the method.
The third purpose of the invention is to provide a lithium battery, which comprises the lithium battery negative electrode material, wherein the lithium battery negative electrode material is prepared from the lithium titanate-titanium dioxide composite material prepared by the method.
The invention has the beneficial effects that: the method of the invention can be used for preparing micron-sized TiO2Synthesis of Li4Ti5O12Material, and in TiO2Surface formation of nanoscale Li4Ti5O12Increasing the surface area of the material, and reducing the Li content of lithium ions and electrons4Ti5O12The transmission distance on the material and the doping generated at the two-phase interface of the lithium titanate-titanium dioxide composite material in the invention lead the prepared Li4Ti5O12The material can be mixed with nano-TiO2Synthetic Li4Ti5O12The material is comparable to the material. The lithium battery cathode material prepared by the invention has good lithium ion mobility, and the rate capability of the prepared lithium battery is good.
Drawings
FIG. 1 is an XRD pattern of LTO-TO-4B before and after annealing;
FIG. 2 is an XRD pattern of LTO-TO-1B, LTO-TO-4B and LTO-TO-6B;
FIG. 3 is an XRD pattern of LTO-TO-4A, LTO-TO-4B and LTO-TO-4C;
FIG. 4 is SEM pictures of (a) LTO-TO-1B, (B) LTO-TO-4B and (c) LTO-TO-6B;
FIG. 5 is SEM pictures of (a) LTO-TO-4A, (B) LTO-TO-4B and (C) LTO-TO-4C;
FIG. 6 is a high magnification SEM image of (a) LTO-TO-4B and (B) LTO-TO-4C;
FIG. 7 is a graph of the rate performance of LTO-TO-1B, LTO-TO-4B and LTO-TO-6B; a graph of rate performance for LTO-TO-4A, LTO-TO-4B and LTO-TO-4C and a graph of cycle life performance for LTO-TO-4B and LTO-TO-4C.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1:
1.0.252g lithium hydroxide monohydrate (LiOH. H)2O, 99%) was dissolved in 15ml of deionized water to form a 0.4M lithium hydroxide solution, 0.599g TiO was added2(98% particle size 1 μm, LiOH. H)2O and TiO2Molar ratio 4:5) into the solution and stirred for 2 h.
2. The resulting solution was transferred to a stainless steel autoclave, sealed and incubated at 180 ℃ for 12 hours.
3. The precipitate was separated by filtration centrifugation, washed with deionized water and ethanol, separated in a high speed centrifuge and then dried in an oven at 60 ℃ for 4 hours.
4. The prepared precursor was calcined in a muffle furnace at 700 deg.C (heating rate 10 deg.C/min) in air for 2 hours TO obtain a LTO-TO-4B sample.
Example 2:
1.0.088g lithium hydroxide monohydrate (LiOH. H)2O, 99%) was dissolved in 15ml of deionized water to form a 0.1M lithium hydroxide solution, 0.149g TiO was added2(98% of a particle size of 1 μm, LiOH. H2O and TiO2Molar ratio 4:5) into the solution and stirred for 2 h.
2. The resulting solution was transferred to a stainless steel autoclave, sealed and incubated at 180 ℃ for 12 hours.
3. The precipitate was separated by filtration centrifugation, washed with deionized water and ethanol, separated in a high speed centrifuge and then dried in an oven at 60 ℃ for 4 hours.
4. The prepared precursor was calcined in a muffle furnace at 700 deg.C (heating rate of 10 deg.C/min) in air for 2 hours TO obtain a LTO-TO-1B sample.
Example 3:
1.0.378g lithium hydroxide monohydrate (LiOH. H)2O, 99%) was dissolved in 15ml of deionized water to form a 0.6M lithium hydroxide solution, 0.899g TiO was added2(98% particle size 1 μm, LiOH. H)2O and TiO2Molar ratio 4:5) into the solution and stirred for 2 h.
2. The resulting solution was transferred to a stainless steel autoclave, sealed and incubated at 180 ℃ for 12 hours.
3. The precipitate was separated by filtration centrifugation, washed with deionized water and ethanol, separated in a high speed centrifuge and then dried in an oven at 60 ℃ for 4 hours.
4. The prepared precursor was calcined in a muffle furnace at 700 deg.C (heating rate 10 deg.C/min) in air for 2 hours TO obtain a LTO-TO-6B sample.
Example 4:
1.0.252g lithium hydroxide monohydrate (LiOH. H)2O, 99%) was dissolved in 15ml of deionized water to form a 0.4M lithium hydroxide solution, 0.599g TiO was added2(98% particle size 1 μm, LiOH. H)2O and TiO2Molar ratio 4:5) into the solution and stirred for 2 h.
2. The resulting solution was transferred to a stainless steel autoclave, sealed and incubated at 180 ℃ for 8 hours.
3. The precipitate was separated by filtration centrifugation, washed with deionized water and ethanol, separated in a high speed centrifuge and then dried in an oven at 60 ℃ for 4 hours.
4. The prepared precursor was calcined in a muffle furnace at 700 deg.C (heating rate 10 deg.C/min) in air for 2 hours TO obtain a LTO-TO-4A sample.
Example 5:
1.0.252g lithium hydroxide monohydrate (LiOH. H)2O, 99%) was dissolved in 15ml of deionized water to form a 0.4M lithium hydroxide solution, 0.599g TiO was added2(98% particle size 1 μm, LiOH. H)2O and TiO2Molar ratio 4:5) into the solution and stirred for 2 h.
2. The resulting solution was transferred to a stainless steel autoclave, sealed and incubated at 180 ℃ for 16 hours.
3. The precipitate was separated by filtration centrifugation, washed with deionized water and ethanol, separated in a high speed centrifuge and then dried in an oven at 60 ℃ for 4 hours.
4. The prepared precursor was calcined in a muffle furnace at 700 deg.C (heating rate 10 deg.C/min) in air for 2 hours TO obtain a LTO-TO-4C sample.
Testing the performance of the lithium titanate-titanium dioxide composite material:
the main measurement methods are XRD, SEM, constant current charge and discharge, EIS and CV. Mainly explore LiOH. H2O concentration (0.1M, 0.4M and 0.6M) and hydrothermal reaction time (8h, 12h and 16h) vs Li4Ti5O12The impact of the generation.
XRD before and after annealing as shown in FIG. 1, LiTiO was formed during hydrothermal reaction2In a subsequent annealing process of LiTiO2And TiO2Reaction to form Li4Ti5O12. FIG. 2 is an XRD pattern of LTO-TO-1B, LTO-TO-4B and LTO-TO-6B, from which it can be seen that there is almost no Li in LTO-TO-1B4Ti5O12The product of LTO-TO-4B is Li4Ti5O12And TiO2Of which the majority is Li4Ti5O12The product of LTO-TO-6B is mostly Li4Ti5O12With only a small amount of TiO2. SEM pictures of LTO-TO-1B and LTO-TO-4B and LTO-TO-6B (as shown in FIG. 4)The results of this study further demonstrate that LTO-TO-1B (FIG. 4a) is composed of 1 μm bulk particles, most of which have smooth surface and only a small fraction of which is 5-10 nm, and that the bulk particles are TiO when combined with XRD2The small particles are Li4Ti5O12，TiO2And LiOH. H2The reaction process of O is LiOH. H2O and TiO2And reacting on the surface. And the surfaces of LTO-TO-4B and LTO-TO-6B (FIGS. 4B and c) are all Li4Ti5O12However, the small particle size of LTO-TO-4B is smaller than that of LTO-TO-6B, which explains the TiO content of LTO-TO-4B2More than LTO-TO-6B, which is consistent with XRD pattern response.
FIG. 3 is an XRD pattern for LTO-TO-4A, LTO-TO-4B and LTO-TO-4C, all products being Li4Ti5O12And TiO2Li of different reaction times4Ti5O12And TiO2In different proportions. By comparing LTO-TO-4A with LTO-TO-4B, it is clear that Li of LTO-TO-4B4Ti5O12Higher contents, indicating an increased progress of the reaction with increasing time, Li of LTO-TO-4B and LTO-TO-4C4Ti5O12The contents are relatively close, which indicates that the hydrothermal reaction is substantially completed after 12 h. SEM images of LTO-TO-4A, LTO-TO-4B and LTO-TO-4C (as shown in FIG. 5), which are consistent with the results of XRD. In a high power SEM (as shown in FIG. 6), Li of LTO-TO-4B4Ti5O12Has a smaller particle size than LTO-TO-4C.
FIG. 7a is a graph showing the charge-discharge rate characteristics of LTO-TO-1B, LTO-TO-4B and LTO-TO-6B, in which the discharge capacity of LTO-TO-4 is 140mAh/g and 90mAh/g at 0.5C and 10C, respectively, which are superior TO 0LTO-TO-1B and LTO-TO-6B, FIG. 7B is a graph of the charge-discharge rate performance of LTO-TO-4A, LTO-TO-4B and LTO-TO-4C, the capacity of LTO-TO-4A is significantly worse than that of LTO-TO-4B and LTO-TO-4C, and the LTO-TO-4B and LTO-TO-4C have relatively close capacities, however, LTO-TO-4B was more stable than LTO-TO-4C at long cycles of 0.5C (as shown in FIG. 7C).
The above results show that Li4Ti5O12/TiO2Li in composite materials4Ti5O12Provide a batteryMain capacity of (3), TiO2The core of (2) mainly fixes Li4Ti5O12The function of (1). The core-shell result has excellent electrochemical performance.
In addition, the invention adopts LiOH. H2O is used as a lithium source, and the characteristic that titanium dioxide is slightly soluble in alkali is utilized, so that the two phases are mixed favorably, and the lithium ion battery has a better effect compared with other lithium sources.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (4)
1. A preparation method of a lithium titanate-titanium dioxide composite material is characterized by comprising the following steps:
(1) 0.252g of lithium hydroxide monohydrate was dissolved in 15ml of deionized water to form a 0.4M lithium hydroxide solution, and 0.599g of TiO was added2Adding the mixture into the solution and stirring for 2 hours;
(2) transferring the obtained solution into a stainless steel autoclave, sealing and preserving heat for 12 hours at 180 ℃;
(3) centrifuging the precipitate by filtration, washing with deionized water and ethanol, separating in a high speed centrifuge, and drying in an oven at 60 deg.C for 4 hr;
(4) calcining the prepared precursor in a muffle furnace at 700 ℃ in air for 2 hours to obtain the lithium titanate-titanium dioxide composite material;
wherein, TiO2With a particle size of 1 μm, lithium hydroxide monohydrate and TiO2The molar ratio was 4: 5.
2. A lithium titanate-titanium dioxide composite material prepared by the process of claim 1.
3. A negative electrode material for a lithium battery, characterized by being prepared from the lithium titanate-titanium dioxide composite material according to claim 2.
4. A lithium battery comprising the negative electrode material for lithium batteries according to claim 3.
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