CN108417824B - Preparation method of high-performance lithium battery cathode material carbon-coated lithium titanate - Google Patents
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Abstract
The invention discloses a preparation method of carbon-coated lithium titanate serving as a high-performance lithium battery cathode material. The method specifically comprises the following steps: dissolving CTAB in isopropanol at room temperature, and uniformly mixing by magnetic stirring; then, dropwise adding tetrabutyl titanate, dropwise adding a lithium hydroxide aqueous solution into the obtained mixed solution, stirring, transferring the mixture into a stainless steel high-pressure kettle, and keeping the temperature at 180 ℃ for 36 hours to obtain a white precipitate; and (3) centrifugally washing, drying in an oven at 85 ℃, calcining the obtained precursor in a tube furnace at 700-750 ℃ for 6h, cooling, and grinding to obtain the target product. According to the invention, CTAB is innovatively selected as a structure directing agent, and lithium titanate Li with narrow grain size is directionally grown4Ti5O12The nano material forms a special structure of carbon-coated lithium titanate, so that the transmission efficiency of lithium ions and electrons of the lithium titanate is remarkably enhanced, and the electrochemical properties of the material such as rate capability, cycle performance and the like are more excellent.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of a high-performance lithium battery cathode material carbon-coated lithium titanate.
Background
The human society develops rapidly with the progress of science and technology, but also causes the problems of environmental pollution, resource exhaustion and the like. Since the 21 st century, while enjoying high-quality life brought about by scientific development, mankind has gradually recognized the importance of developing new clean energy. Among many new clean energy sources, lithium ion batteries have attracted extensive attention of researchers due to their outstanding advantages of small size, light weight, high energy density, good cycle stability, small self-discharge, no memory effect, safety, reliability, no pollution, and the like.
The lithium ion battery cathode material should be favored by researchers as an important factor for improving the energy, rate capability and cycle life of the battery. In lithium ion batteries, the developed negative electrode materials mainly include carbon negative electrode materials, germanium-based negative electrode materials, silicon-based negative electrode materials, titanium-based negative electrode materials (Li)4Ti5O12) Etc. and titanium-based negative electrode material (Li)4Ti5O12) Has attracted the attention of researchers due to its inherent properties, spinel lithium titanate (Li)4Ti5O12) The material has a flat and wide charge-discharge platform at 1.55V (vs. Li/Li +), and meanwhile, the volume of the material is changed by only 0.2% in the charge-discharge process, so that the material is a 'zero-strain' anode material, and has excellent stability. Spinel lithium titanate (Li)4Ti5O12) The method has two serious defects of poor conductivity and low transmission efficiency of lithium ions and electrons, and researchers modify and optimize the lithium ions and the electrons around the two defects. The modification optimization method of the spinel lithium titanate cathode material commonly adopted at present comprises the steps of nano shortening Li+And the transport distance of electrons inside the material; the preparation of composite material system to build conductive network and increase Li+And the transport capacity of electrons; the doping modification is optimized, the electrode polarization of the material under high multiplying power is reduced, the electron transport capacity of the material is improved, and the like.
With the development of social economy and the progress of civilization, the demand of people on energy is increased day by day, and the development of novel green energy is reluctant. The lithium ion battery as a green high-efficiency energy storage material arouses extensive research interest of scientific researchers. The lithium ion battery cathode material is one of the keys for ensuring high specific energy and cycling stability of the lithium ion electrode. Some new titanium-based negative electrode materials (e.g. Li)4Ti5O12) Has attracted the wide attention and great research interest of people, is hopeful to realize commercialization, and is applied to the next generation of high-performance lithium ion battery, thereby promoting the non-performance of the lithium ion batteryThe development is interrupted, and the method contributes to relieving the energy crisis and promoting the civilization development of human beings.
Disclosure of Invention
In order to solve the problem of low transmission efficiency of lithium ions and electrons in lithium titanate serving as a negative electrode material of a lithium ion battery, the invention aims to provide a preparation method of carbon-coated lithium titanate serving as a negative electrode material of a high-performance lithium battery, so as to further improve the electrochemical performance of the carbon-coated lithium titanate.
The technical scheme adopted by the invention is as follows: a preparation method of carbon-coated lithium titanate as a high-performance lithium battery negative electrode material comprises the following steps:
1) dissolving Cetyl Trimethyl Ammonium Bromide (CTAB) in isopropanol at room temperature, magnetically stirring, uniformly mixing, and adding tetrabutyl titanate to obtain a mixed solution;
2) adding a lithium hydroxide aqueous solution into the mixed solution obtained in the step 1), stirring for 4-5 h, transferring the reaction solution into a stainless steel high-pressure autoclave, reacting for 36-45 h at 175-185 ℃, obtaining a white precipitate, centrifugally washing, and drying in an oven at 85 ℃ to obtain a precursor;
3) and (3) placing the precursor obtained in the step 2) into a tube furnace, calcining for 6-7 h at 600-750 ℃ in a nitrogen atmosphere, naturally cooling to room temperature, and grinding to obtain a target product.
According to the preparation method, the lithium hydroxide and the tetrabutyl titanate are mixed according to the lithium-titanium molar ratio of 4.5: 5.
In the preparation method, the tetrabutyl titanate and the lithium hydroxide aqueous solution are added dropwise.
According to the preparation method, the calcining temperature is 700-750 ℃.
The invention has the beneficial effects that:
the invention provides a preparation method of high-performance lithium battery cathode material carbon-coated lithium titanate, which adopts an isopropanol-water composite solvothermal method and uses tetrabutyl titanate and LiOH & H2Taking O as a raw material, taking isopropanol and water as solvents, and reacting for 36-45 h at the temperature of 175-185 ℃ to obtain a precursor; sintering the precursor at high temperature in nitrogen atmosphere to obtain the target product Li4Ti5O12and/C. Nano Li prepared by the method4Ti5O12the/C material not only solves the problem of low transmission efficiency of lithium ions and electrons of lithium titanate on the premise of keeping the excellent characteristics of LTO, but also particularly, the microstructure of the material further increases the specific surface area of the material, thereby improving the electrochemical performance of the material. And the method is synthesized by one step by adopting a very simple isopropanol-water composite solvothermal method, is particularly favorable for realizing commercialization of LTO electrode materials and promoting the development process of lithium ion battery cathode materials.
According to the invention, CTAB is innovatively selected as a structure directing agent in the preparation process, and lithium titanate Li with narrow grain size is directionally grown4Ti5O12The prepared nano material has larger specific surface area and more active contact sites when contacting with the electrolyte. Meanwhile, CTAB provides a proper amount of carbon source for the synthesis of the composite material, and trace carbon is deposited on the surface of lithium titanate in the process of calcining in an inert atmosphere, so that a special structure of carbon-coated lithium titanate is formed, the transmission efficiency of lithium ions and electrons of lithium titanate is remarkably enhanced, and the electrochemical properties of the material such as rate capability, cycle performance and the like are more excellent.
Drawings
FIG. 1 shows Li obtained by calcining at 700-750 deg.C4Ti5O12XRD pattern of/C.
FIG. 2 shows Li obtained by calcining at 600-650 deg.C4Ti5O12XRD pattern of/C.
FIG. 3 shows Li obtained by calcining at 700-750 deg.C4Ti5O12SEM image of/C;
wherein, a: 1 μm; b: 500 nm.
Detailed Description
The invention is further explained below with reference to specific embodiments, but is not intended to limit the scope of protection of the invention.
The invention provides a preparation method of carbon-coated lithium titanate as a high-performance lithium battery cathode material, which comprises the following steps:
1) dissolving Cetyl Trimethyl Ammonium Bromide (CTAB) in isopropanol at room temperature, magnetically stirring for 4h, and mixing uniformly; then, dropwise adding tetrabutyl titanate to obtain a mixed solution;
2) dissolving lithium hydroxide in deionized water, and obtaining a lithium hydroxide aqueous solution after completely dissolving the lithium hydroxide by magnetic stirring. Dropwise adding a lithium hydroxide aqueous solution into the mixed solution obtained in the step 1), stirring for 5 hours, transferring the mixture into a stainless steel autoclave, reacting for 36-45 hours at 175-185 ℃, and carrying out hydrothermal treatment to obtain a white precipitate; centrifugally washing for 5 times, and drying in an oven at 85 ℃ to obtain a precursor;
3) putting the precursor obtained in the step 2) into a tube furnace, calcining for 6 hours at the temperature of 700-750 ℃ and the temperature of 600-650 ℃, naturally cooling to room temperature, grinding to obtain target products Li4Ti5O12/C。
Wherein, in order to make the electrochemical performance of the prepared material more excellent, the amount of CTAB in the step 1) is proper, namely 10mmol of tetrabutyl titanate and 9mmol of lithium hydroxide are added per 0.2g of CTAB. The molar ratio of lithium to titanium was 4.5:5, and lithium was required to be excessive because the lithium source was lost during the high-temperature calcination in step 3), and if lithium was not excessive, impurity TiO was formed2. Step 3) high-temperature calcination in nitrogen atmosphere is carried out, so that the precursor is converted into spinel lithium titanate Li under the high-temperature condition4Ti5O12And the anode material and CTAB can be converted into a carbon source in an inert atmosphere.
In order to ensure that the raw materials lithium hydroxide and tetrabutyl titanate are sufficiently reacted, as a modification of the technical solution, lithium hydroxide is added in a dropwise addition manner.
Wherein, in the step 2), LiOH & H2And (3) stirring the O in the deionized water, preferably magnetically stirring, so as to control the stirring speed and improve the uniformity.
The calcination temperature in the step 3) is preferably 700-750 ℃.
Example 1
The preparation method of the high-performance lithium battery cathode material carbon-coated lithium titanate comprises the following steps:
1) dissolving 0.2g of hexadecyl trimethyl ammonium bromide (CTAB) in 30mL of isopropanol at room temperature, magnetically stirring for 4 hours, and uniformly mixing; then, dropwise adding 10mmol of tetrabutyl titanate to obtain a mixed solution;
2) and (3) dissolving 9mmol of lithium hydroxide in 15mL of deionized water, and obtaining a lithium hydroxide aqueous solution after completely dissolving by magnetic stirring. Dropwise adding a lithium hydroxide aqueous solution into the mixed solution obtained in the step 1), stirring for 5h, transferring the mixture into a 100mL stainless steel autoclave, reacting for 36h at 175-185 ℃, and carrying out hydrothermal treatment to obtain a white precipitate; centrifugally washing for 5 times, and drying in an oven at 85 ℃ to obtain a precursor;
3) putting the precursor obtained in the step 2) into a tube furnace, calcining for 6 hours at the temperature of 600-650 ℃, naturally cooling to room temperature, and grinding to obtain the target product Li4Ti5O12/C。
Example 2
The preparation method of the high-performance lithium battery cathode material carbon-coated lithium titanate comprises the following steps:
1) dissolving 0.2g of hexadecyl trimethyl ammonium bromide (CTAB) in 30mL of isopropanol at room temperature, magnetically stirring for 4 hours, and uniformly mixing; then, dropwise adding 10mmol of tetrabutyl titanate to obtain a mixed solution;
2) and (3) dissolving 9mmol of lithium hydroxide in 15mL of deionized water, and obtaining a lithium hydroxide aqueous solution after completely dissolving by magnetic stirring. Dropwise adding a lithium hydroxide aqueous solution into the mixed solution obtained in the step 1), stirring for 5h, transferring the mixture into a 100mL stainless steel autoclave, reacting for 36h at 175-185 ℃, and carrying out hydrothermal treatment to obtain a white precipitate; centrifugally washing for 5 times, and drying in an oven at 85 ℃ to obtain a precursor;
3) putting the precursor obtained in the step 2) into a tube furnace, calcining for 6 hours at the temperature of 700-750 ℃, naturally cooling to room temperature, and grinding to obtain the target product Li4Ti5O12/C。
Li obtained in example 1 and example 24Ti5O12XRD and SEM detection are carried out on the/C, and the results are shown in figure 1, figure 2 and figure 3.
As can be seen from FIG. 1, the target product Li obtained in example 14Ti5O12The purity of the/C is high, the XRD diffraction peak is sharp, and no other miscellaneous peak appears compared with the lithium titanate standard card (JCPDS card number: 49-0207).
As can be seen from FIG. 2, the target product Li obtained in example 24Ti5O12C, the spectrum shows some TiO2Impurity peaks, XRD diffraction peaks are also less sharp than those of fig. 1.
As can be seen from FIG. 3, the target product Li obtained in example 14Ti5O12And C, the particle size is narrow, and the morphology is regular.
Example 3
The electrochemical performance of the button cell was measured by using the materials obtained in examples 1 and 2 and a commercially available LTO material as a negative electrode material and a lithium plate as a counter electrode, respectively, and the results are shown in table 1.
TABLE 1 comparison of electrochemical Properties of different cathode materials (Charge-discharge multiplying factor 1C)
As can be seen from Table 1, compared with the common LTO negative electrode material, the high-performance lithium battery negative electrode material lithium titanate Li synthesized by the method of the invention4Ti5O12The electrochemical performance of the/C is obviously improved, and the electrochemical performance of the material obtained by calcining at the temperature of 700-750 ℃ is far higher than that of the material obtained by calcining at the temperature of 600-650 ℃ and has good electrochemical performance; CTAB is newly selected as a structure directing agent of the material in the preparation process, and lithium titanate Li with narrow grain diameter is directionally grown4Ti5O12The nano material has a larger specific surface area, has more active contact sites when contacting with electrolyte, simultaneously provides a proper amount of carbon source for the synthesis of the composite material, and trace carbon is deposited on the surface of lithium titanate in the process of calcining in an inert atmosphere, so that a special structure of carbon-coated lithium titanate is formedThe transmission efficiency of lithium ions and electrons of the lithium titanate is obviously enhanced, and further the electrochemical properties of the material such as rate capability, cycle performance and the like are more excellent.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. A preparation method of carbon-coated lithium titanate as a high-performance lithium battery cathode material is characterized by comprising the following steps:
1) dissolving hexadecyl trimethyl ammonium bromide in isopropanol at room temperature, magnetically stirring, uniformly mixing, and then dropwise adding tetrabutyl titanate to obtain a mixed solution;
2) dropwise adding a lithium hydroxide aqueous solution into the mixed solution obtained in the step 1), stirring for 4-5 h, transferring the reaction solution into a stainless steel high-pressure kettle, reacting for 36-45 h at 175-185 ℃, obtaining a white precipitate, centrifugally washing, and drying in an oven at 85 ℃ to obtain a precursor;
adding 10mmol of tetrabutyl titanate and 9mmol of lithium hydroxide into each 0.2g of hexadecyl trimethyl ammonium bromide;
3) and (3) placing the precursor obtained in the step 2) into a tube furnace, calcining for 6-7 h at 600-750 ℃ in a nitrogen atmosphere, naturally cooling to room temperature, and grinding to obtain a target product.
2. The method according to claim 1, wherein the lithium hydroxide and tetrabutyl titanate are compounded in a molar ratio of lithium to titanium of 4.5: 5.
3. The method according to claim 1, wherein the calcination temperature is 700 to 750 ℃.
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| CN109148858B (en) * | 2018-08-29 | 2021-12-07 | 西安交通大学苏州研究院 | Lithium titanate-titanium dioxide composite material and preparation method and application thereof |
| CN111653748B (en) * | 2020-06-04 | 2021-08-06 | 松山湖材料实验室 | Ge-GeO2-TiO2Preparation method of-C nanocomposite material, product and application thereof |
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