CN112038625A - Lithium titanate negative electrode material and preparation method thereof - Google Patents
Lithium titanate negative electrode material and preparation method thereof Download PDFInfo
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- 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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- C01G23/005—Alkali titanates
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Abstract
The invention discloses a lithium titanate negative electrode material and a preparation method thereof, relating to the technical field of lithium ion batteries and comprising the following steps: adding a titanium source and a lithium source into an anhydrous alcohol solution, adding styrene, divinyl and an initiator, and mixing to obtain a mixed solution; soaking the porous ceramic in the mixed solution; taking out the soaked porous ceramic, heating the porous ceramic by microwave until the porous ceramic is gelated and combusted, and separating the porous ceramic to obtain lithium titanate precursor powder; and sintering the lithium titanate precursor powder to obtain the lithium titanate powder. The lithium titanate powder prepared by the invention is fluffy and easy to crush, has small particle size, narrow distribution, high activity, excellent electrochemical performance, short synthesis time of the whole preparation process and high yield.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a lithium titanate negative electrode material and a preparation method thereof.
Background
Most of the current commercialized lithium ion battery negative electrode materials adopt various carbon materials, but the potential of the carbon negative electrode is very close to the standard potential of lithium, when the battery is overcharged, metal lithium may precipitate on the surface of the carbon electrode to form dendrite to cause safety problems,and the quick charge and discharge capacity is not strong, so that the device is not suitable for equipment with instantaneous strong current. The electrode potential of the spinel-structured lithium titanate with respect to lithium metal was 1.55v (Li/Li)+) The theoretical capacity was 175 mAh/g. Li+The insertion and the extraction of the lithium ion battery have almost no influence on the structure of the material, and have the excellent characteristics of excellent cycle performance, stable discharge voltage, high lithium insertion potential, difficult metallic lithium precipitation, high coulombic efficiency, wide material source, cleanness, environmental protection and the like, and can be used in the stable voltage range of most liquid electrolytes. Lithium titanate has the characteristics of more charging times, faster charging process, higher safety and the like required by the next generation of lithium ion batteries. In addition, lithium titanate also has an obvious charge-discharge platform, the platform capacity can reach more than 90% of the discharge capacity, and the lithium titanate has the characteristics of obvious voltage mutation and the like when the charge-discharge is finished.
The method for preparing the lithium titanate with the spinel structure mainly adopts high-temperature solid-phase synthesis, has the advantages of simple process and easy realization of industrialization, but has the problems of insufficient batch stability due to the fact that reactants need to be mixed for a long time and are not easy to be mixed uniformly, and the obtained product has large particle size, uneven distribution and irregular shape. The spinel-structured lithium titanate can be directly synthesized by a hydrothermal method and a spray pyrolysis method, and the morphology and the particle size of the material are relatively easy to control, but the two methods have high requirements on equipment, are difficult to operate and are difficult to realize industrialization. The product prepared by the sol-gel method has high purity, good uniformity and low heat treatment temperature, but the method has long production period and low yield and is not easy for industrial production.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a lithium titanate negative electrode material and a preparation method thereof, and the prepared lithium titanate powder is fluffy, easy to crush, small in particle size, narrow in distribution, high in activity and excellent in electrochemical performance.
The preparation method of the lithium titanate negative electrode material provided by the invention comprises the following steps:
s1, adding a titanium source and a lithium source into the anhydrous alcohol solution, adding styrene, divinyl and an initiator, and mixing to obtain a mixed solution;
s2, placing the porous ceramic in the mixed solution for soaking;
s3, taking out the soaked porous ceramic, heating the porous ceramic by microwave until gelation and combustion are achieved, and then separating the porous ceramic to obtain lithium titanate precursor powder;
and S4, sintering the lithium titanate precursor powder to obtain the lithium titanate powder.
Preferably, in S1, the titanium source is titanium tetrachloride or tetrabutyl titanate.
Preferably, in S1, the lithium source is any one of lithium chloride, lithium nitrate, and lithium oxalate.
Preferably, in S1, the anhydrous alcohol solution is methanol or ethanol; preferably, the initiator is tert-butyl peroxybenzoate.
Preferably, in S1, the titanium source and the lithium source are in molar ratio nLi：nTi4: 4.5 to 5.0; preferably, the weight ratio of divinylbenzene to styrene is 1: 2-10; preferably, the weight concentration of the anhydrous alcohol solution of styrene and divinylbenzene is 1-5%; preferably, the addition amount of the initiator is 0.05-0.2% of the total weight of the divinylbenzene and the styrene.
Preferably, in S2, the material of the porous ceramic is any one of zirconia, alumina, silicon carbide, silicon nitride, and zirconium diboride; preferably, the porous ceramic has a pore diameter of 25 to 50 μm and a porosity of 40 to 60%.
Preferably, in S2, soaking for 3-5 min.
Preferably, in S3, microwave heating is carried out to 80-85 ℃; preferably, the microwave power is 400-600W.
Preferably, in S4, the sintering is carried out in an air atmosphere at 700-900 ℃ for 5-10 h.
The invention also provides a lithium titanate negative electrode material prepared by the method.
Has the advantages that: in the invention, styrene and divinyl benzene are subjected to in-situ polymerization reaction to form a polymer network to fix metal ions lithium and titanium, and the raw materials can be uniformly mixed at a molecular level; the porous ceramic has a multi-wall three-dimensional cross structure, can well absorb reactant solution in a micron-sized cavity of the porous ceramic, is heated uniformly by microwave heating, avoids gel aggregates from appearing, and avoids the injection and loss of reactants in the combustion process because the combustion reaction is limited in holes along with higher temperature. The lithium titanate powder prepared by the invention is fluffy and easy to crush, has small particle size, narrow distribution, high activity, excellent electrochemical performance, short synthesis time of the whole preparation process and high yield.
Drawings
FIG. 1 is an SEM photograph of a lithium titanate powder prepared in example 1 of the present invention;
FIG. 2 is an XRD pattern of lithium titanate powder prepared in example 1 of the present invention;
FIG. 3 is a graph showing the charge and discharge curves of the lithium titanate powder prepared in example 1 of the present invention as a negative electrode material; wherein a is 0.2C, b, 1C, C, 3C, d, 5C, e and 10C.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
(1) Dissolving styrene and divinylbenzene in absolute ethyl alcohol, uniformly stirring, adding tert-butyl peroxybenzoate, and uniformly stirring to obtain a solution A; wherein, the sum of the weight concentrations of the styrene and the divinyl benzene in the solution A is 1%, and the weight ratio of the styrene to the divinyl benzene is 2: 1, adding the tert-butyl peroxybenzoate in an amount which is 0.05 percent of the sum of the weight of the divinylbenzene and the styrene;
(2) adding titanium tetrachloride and lithium nitrate into an absolute ethyl alcohol solution, and uniformly stirring to obtain a solution B; wherein, the concentration of the metal ions in the solution B is 0.05mol/L, nLi：nTi＝4：4.5；
(3) Mixing the solution A and the solution B in proportion to obtain a mixed solution; wherein the weight sum of styrene and divinylbenzene in solution A: metal oxide (in Li) in solution B4Ti5O12Calculated) is 1: 5;
(4) soaking the alumina porous ceramic with the aperture of 25 microns and the porosity of 60% in the mixed solution for 3min, taking out, heating to 80 ℃ by using microwave with the microwave power of 400W until the soaking solution is gradually gelated and then burns, separating out the porous ceramic, and collecting lithium titanate precursor powder;
(5) heating the lithium titanate precursor powder from room temperature to 550 ℃ at the heating rate of 3 ℃/min in the air atmosphere, preserving heat for 5h to decompose part of carbonate in the solution, heating to 700 ℃ at the heating rate of 2 ℃/min, preserving heat for 5h, and naturally cooling to room temperature to obtain the required lithium titanate powder.
FIG. 1 is an SEM of the product obtained in this example, which shows that the primary particle size distribution is 200-500nm, which illustrates that the obtained product has a small particle size and a narrow particle size distribution; FIG. 2 is an XRD of the product obtained in this example, which shows that the diffraction peak is sharp, indicating that the obtained product is a single lithium titanate phase and the product is well crystallized; fig. 3 is a charge-discharge curve diagram of the product obtained in the present embodiment as a negative electrode material, and the discharge performance is excellent at 0.2C, 1C, 3C, 5C, and 10C, especially the rate performance, where the discharge capacity at 0.2C is greater than 165mAh/g, the discharge capacity at 3C is greater than 155mAh/g, and the discharge capacity at 10C is greater than 135 mAh/g.
Example 2
(1) Dissolving styrene and divinylbenzene in absolute ethyl alcohol, uniformly stirring, adding tert-butyl peroxybenzoate, and uniformly stirring to obtain a solution A; wherein, the sum of the weight concentrations of the styrene and the divinyl benzene in the solution A is 5%, and the weight ratio of the styrene to the divinyl benzene is 10: 1, adding the tert-butyl peroxybenzoate in an amount which is 0.2 percent of the sum of the weight of the divinylbenzene and the styrene;
(2) adding titanium tetrachloride and lithium nitrate into an absolute ethyl alcohol solution, and uniformly stirring to obtain a solution B; wherein, the concentration of the metal ions in the solution B is 0.05mol/L, nLi：nTi＝4：5.0；
(3) Mixing the solution A and the solution B in proportion to obtain a mixed solution; wherein the weight sum of styrene and divinylbenzene in solution A: metal oxide (in Li) in solution B4Ti5O12Calculated) is 1: 5;
(4) soaking the alumina porous ceramic with the aperture of 50 microns and the porosity of 40% in the mixed solution for 5min, taking out, heating to 85 ℃ by using microwave with the microwave power of 600W until the soaking solution is gradually gelatinized and then burns, separating out the porous ceramic, and collecting lithium titanate precursor powder;
(5) heating the lithium titanate precursor powder from room temperature to 550 ℃ at the heating rate of 3 ℃/min in the air atmosphere, preserving heat for 5h, then heating to 900 ℃ at the heating rate of 2 ℃/min, preserving heat for 10h, and then naturally cooling to room temperature to obtain the required lithium titanate powder.
Example 3
(1) Dissolving styrene and divinylbenzene in absolute ethyl alcohol, uniformly stirring, adding tert-butyl peroxybenzoate, and uniformly stirring to obtain a solution A; wherein, the sum of the weight concentrations of the styrene and the divinyl benzene in the solution A is 2.5%, and the weight ratio of the styrene to the divinyl benzene is 4: 1, the addition amount of tert-butyl peroxybenzoate is 0.1 percent of the sum of the weight of divinylbenzene and styrene;
(2) adding titanium tetrachloride and lithium nitrate into an absolute ethyl alcohol solution, and uniformly stirring to obtain a solution B; wherein, the concentration of the metal ions in the solution B is 0.05mol/L, nLi：nTi＝4：4.7；
(3) Mixing the solution A and the solution B in proportion to obtain a mixed solution; wherein the weight sum of styrene and divinylbenzene in solution A: metal oxide (in Li) in solution B4Ti5O12Calculated) is 1: 5;
(4) soaking the alumina porous ceramic with the aperture of 40 microns and the porosity of 50% in the mixed solution for 4min, taking out, heating to 80 ℃ by using microwave with the microwave power of 500W until the soaking solution is gradually gelated and then burns, separating out the porous ceramic, and collecting lithium titanate precursor powder;
(5) heating the lithium titanate precursor powder from room temperature to 550 ℃ at the heating rate of 3 ℃/min in the air atmosphere, preserving heat for 5h, then heating to 700 ℃ at the heating rate of 2 ℃/min, preserving heat for 10h, and then naturally cooling to room temperature to obtain the required lithium titanate powder.
Example 4
(1) Dissolving styrene and divinylbenzene in absolute ethyl alcohol, uniformly stirring, adding tert-butyl peroxybenzoate, and uniformly stirring to obtain a solution A; wherein, the sum of the weight concentrations of the styrene and the divinyl benzene in the solution A is 3.5%, and the weight ratio of the styrene to the divinyl benzene is 7: 1, the addition amount of tert-butyl peroxybenzoate is 0.15 percent of the sum of the weight of divinylbenzene and styrene;
(2) adding titanium tetrachloride and lithium nitrate into an absolute ethyl alcohol solution, and uniformly stirring to obtain a solution B; wherein, the concentration of the metal ions in the solution B is 0.05mol/L, nLi：nTi＝4：4.8；
(3) Mixing the solution A and the solution B in proportion to obtain a mixed solution; wherein the weight sum of styrene and divinylbenzene in solution A: metal oxide (in Li) in solution B4Ti5O12Calculated) is 1: 5;
(4) soaking the alumina porous ceramic with the aperture of 40 microns and the porosity of 50% in the mixed solution for 5min, taking out, heating to 85 ℃ by using microwave with the microwave power of 500W until the soaking solution is gradually gelatinized and then burns, separating out the porous ceramic, and collecting lithium titanate precursor powder;
(5) heating the lithium titanate precursor powder from room temperature to 550 ℃ at the heating rate of 3 ℃/min in the air atmosphere, preserving heat for 5h, then heating to 900 ℃ at the heating rate of 2 ℃/min, preserving heat for 5h, and then naturally cooling to room temperature to obtain the required lithium titanate powder.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A preparation method of a lithium titanate negative electrode material is characterized by comprising the following steps:
s1, adding a titanium source and a lithium source into the anhydrous alcohol solution, adding styrene, divinyl and an initiator, and mixing to obtain a mixed solution;
s2, placing the porous ceramic in the mixed solution for soaking;
s3, taking out the soaked porous ceramic, heating the porous ceramic by microwave until gelation and combustion are achieved, and then separating the porous ceramic to obtain lithium titanate precursor powder;
and S4, sintering the lithium titanate precursor powder to obtain the lithium titanate powder.
2. The method for preparing a lithium titanate negative electrode material according to claim 1, wherein in S1, the titanium source is titanium tetrachloride or tetrabutyl titanate.
3. The method for preparing a lithium titanate negative electrode material according to claim 1 or 2, wherein in S1, the lithium source is any one of lithium chloride, lithium nitrate, and lithium oxalate.
4. The method for preparing a lithium titanate negative electrode material according to any one of claims 1 to 3, wherein in S1, the anhydrous alcohol solution is methanol or ethanol; preferably, the initiator is tert-butyl peroxybenzoate.
5. The method for preparing a lithium titanate negative electrode material as claimed in any one of claims 1 to 4, wherein in S1, the molar ratio n of the titanium source to the lithium source isLi：nTi4: 4.5 to 5.0; preferably, the weight ratio of divinylbenzene to styrene is 1: 2-10; preferably, the weight concentration of the anhydrous alcohol solution of styrene and divinylbenzene is 1-5%; preferably, the addition amount of the initiator is 0.05-0.2% of the total weight of the divinylbenzene and the styrene.
6. The method for preparing a lithium titanate negative electrode material according to any one of claims 1 to 5, wherein in S2, the porous ceramic is made of any one of zirconia, alumina, silicon carbide, silicon nitride and zirconium diboride; preferably, the porous ceramic has a pore diameter of 25 to 50 μm and a porosity of 40 to 60%.
7. The method for preparing a lithium titanate negative electrode material according to any one of claims 1 to 6, wherein in S2, soaking is performed for 3-5 min.
8. The method for preparing the lithium titanate negative electrode material as claimed in any one of claims 1 to 7, wherein in S3, microwave heating is carried out to 80-85 ℃; preferably, the microwave power is 400-600W.
9. The method for preparing a lithium titanate negative electrode material as claimed in any one of claims 1 to 8, wherein in S4, the sintering is performed in an air atmosphere at 700 to 900 ℃ for 5 to 10 hours.
10. A lithium titanate negative electrode material prepared based on the method of any one of claims 1-9.
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