CN112670446A - Lithium titanate electrode capable of inhibiting gas production and preparation method thereof - Google Patents
Lithium titanate electrode capable of inhibiting gas production and preparation method thereof Download PDFInfo
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- CN112670446A CN112670446A CN202011538469.2A CN202011538469A CN112670446A CN 112670446 A CN112670446 A CN 112670446A CN 202011538469 A CN202011538469 A CN 202011538469A CN 112670446 A CN112670446 A CN 112670446A
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Abstract
The invention belongs to the technical field of energy and new materials, and discloses a lithium titanate electrode for inhibiting gas production and a preparation method thereof. The electrode is composed of lithium titanate and lithium fluoride and lithium phosphate attached to the surface of the lithium titanate. The lithium fluoride and the lithium phosphate are electrochemical inert, the lithium ion conductivity is high, and the lithium fluoride and the lithium phosphate cooperatively coat lithium titanate to form a compact coating layer, so that catalytic active points on the surface of a lithium titanate electrode are effectively shielded, and the problem of gas generation of the lithium titanate electrode in the use process is solved. According to the invention, a coprecipitation method is adopted, so that lithium fluoride and lithium phosphate are uniformly coated on the surface of lithium titanate, and then heat treatment is carried out, so that the lithium phosphate, the lithium fluoride and the lithium titanate are more tightly combined. The lithium titanate electrode coated by the lithium fluoride and the lithium phosphate can effectively inhibit the gas production of the lithium titanate electrode. The preparation method is simple and convenient, has low cost and is beneficial to large-scale popularization and application.
Description
Technical Field
The invention relates to the technical field of energy and new materials, in particular to a lithium titanate electrode for inhibiting gas production and a preparation method thereof.
Background
Spinel type lithium titanate (Li)4Ti5O12LTO) as a lithium ion battery cathode material has long cycle lifeThe lithium ion battery cathode material has the characteristics of high safety performance, environmental friendliness and the like, is considered to be one of the most promising power lithium ion battery cathode materials, and thus has attracted extensive attention. LTO has two distinct advantages over other anode materials: (1) the charging and discharging voltage platform is 1.55V (vs. Li +/Li), the reduction and decomposition of the common electrolyte on the surface can be avoided, and the safety is high; (2) the electrode material is 'zero strain' electrode material, the unit cell has almost no volume change in the process of lithium ion de-intercalation, and the cycle performance is excellent.
However, LTO has the problem of gas expansion as the negative electrode material of the lithium ion battery in the practical use process. There are several known causes of battery gassing in which LTO is the negative electrode. Novak and Belharouak et al [ J.electrochem. Soc.,2015,162(6): A870-A876; j.electrochem. Soc.,2012,159(8) A1165-A1170] considers that moisture is introduced in the battery assembly process, so that the flatulence behavior of the LTO negative electrode material is caused by the decomposition of water in the charging and discharging processes; wu et al [ J.Power Sources,2013,237: 285-; he et al [ J.Power Sources,2012,202:253-261] suggest that the main cause of LTO gassing is gas evolution due to the presence of catalytically active sites on the surface and interfacial reaction with the electrolyte. Practical application shows that the charged soft package battery with LTO as the negative electrode also has gas production behavior in a storage state, so that the existence of interface reaction between LTO and electrolyte is considered to be more convincing to cause gas expansion.
The research of the prior art shows that the inflation of the LTO can be effectively inhibited by modifying (coating) the surface of the LTO or modifying an electrolyte additive and the like through an inert material, wherein the more common method is to coat a carbon film on the surface of the LTO or coat other inert materials such as alumina and the like. However, the surface modification of the LTO in the prior art is limited to use of a single material, and the inhibition of gas production by the LTO is limited. Therefore, there is a need to research a lithium titanate composite electrode material modified by various materials.
Disclosure of Invention
The invention aims to provide a lithium titanate electrode for inhibiting gas generation and a preparation method thereof, so as to solve the gas generation behavior when LTO is applied to a lithium ion battery cathode material.
The purpose of the invention is realized by the following principle: ammonium fluoride, lithium hydroxide and ammonium dihydrogen phosphate are used as raw materials, a coprecipitation method is adopted, fluoride ions, phosphate ions and lithium ions can form lithium fluoride and lithium phosphate which are insoluble in water, when lithium titanate particles are added into the precursor solution, the formed lithium fluoride and lithium phosphate can use lithium titanate as seed crystals to uniformly grow on the surfaces of the lithium fluoride and lithium phosphate, and the surfaces of the formed lithium fluoride and lithium phosphate and lithium titanate can be more tightly combined together through further heat treatment. Due to the synergistic effect of the lithium fluoride and the lithium phosphate, a compact coating layer can be formed on the surface of the lithium titanate, and catalytic active points on the surface of the lithium titanate are better shielded, so that the problem of gas generation expansion of the lithium titanate negative electrode material is solved.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a lithium titanate electrode for inhibiting gas generation, which consists of lithium titanate, lithium phosphate and lithium fluoride tightly attached to the surface of the lithium titanate electrode.
Preferably, in the above lithium titanate electrode for suppressing gas evolution, the lithium titanate is submicron in size and 100nm to 1 μm in size.
Preferably, in the above lithium titanate electrode for suppressing gas evolution, lithium phosphate and lithium fluoride are mixed together and coated on the surface of lithium titanate, so that a dense coating layer can be formed.
Preferably, in the above lithium titanate electrode for inhibiting gas evolution, the mass percentage of lithium phosphate and lithium fluoride in the lithium titanate electrode is 0.1-3%.
Preferably, in the above lithium titanate electrode for suppressing gas evolution, the mass ratio of lithium phosphate to lithium fluoride in the lithium titanate electrode is 1: 10-10: 1.
the invention also provides a preparation method of the lithium titanate electrode for inhibiting gas generation, which comprises the following steps:
(1) dissolving ammonium dihydrogen phosphate and ammonium fluoride in deionized water to form a mixed solution with the concentration of 0.01-0.1 mol/L;
(2) adding lithium titanate into the mixed solution obtained in the step (1), and fully stirring to form a suspension;
(3) slowly dripping 0.04mol/L-0.4mol/L lithium hydroxide solution into the suspension obtained in the step (2), fully stirring, and filtering to obtain filter residue;
(4) repeatedly washing the filter residue obtained in the step (3) with deionized water until the existence of ammonium ions and lithium ions cannot be detected in the washing liquid;
(5) drying the product obtained in the step (4), and fully grinding;
(6) and (4) carrying out heat treatment on the product obtained in the step (5) in an inert atmosphere at the temperature of 300-600 ℃ for 2-6h to obtain the lithium titanate electrode which is coated by the lithium fluoride and the lithium phosphate.
Preferably, in the above method for preparing a lithium titanate electrode with suppressed gassing, the dropping speed of the lithium hydroxide solution in step (3) is 0.1-1 mL/min.
Preferably, in the above method for preparing a lithium titanate electrode with suppressed gas evolution, the heat treatment temperature in step (6) is 400 ℃ and the heat treatment time is 2 hours.
Preferably, in the above method for preparing a lithium titanate electrode with suppressed gassing, the inert atmosphere for the heat treatment in step (6) is nitrogen or argon, preferably nitrogen.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
according to the invention, co-modification of the lithium titanate by lithium phosphate and lithium fluoride is realized by adopting a co-precipitation method and a heat treatment means, and a compact coating layer can be formed on the surface of the lithium titanate by synergistic mixing of the lithium fluoride and the lithium phosphate, so that catalytic active sites on the surface of the lithium titanate are better shielded, and the effect of effectively inhibiting the gas production of the lithium titanate cathode material is achieved. The preparation method is simple and convenient, has low cost and is beneficial to large-scale popularization and application.
Drawings
Fig. 1 is a TEM image of a gas evolution-inhibited lithium titanate electrode co-coated with lithium phosphate and lithium fluoride in example 1.
Fig. 2 is a TEM image of an uncoated lithium titanate electrode in comparative example 1.
Fig. 3 is a comparison of gas evolution in a pouch cell assembled from the lithium titanate electrode co-coated with lithium phosphate and lithium fluoride of example 1 and the uncoated lithium titanate electrode of comparative example 1.
Fig. 4 is an SEM image after cycling of the gas production-inhibiting lithium titanate electrode co-coated with lithium phosphate and lithium fluoride of example 1.
Fig. 5 is an SEM image of the uncoated lithium titanate electrode of comparative example 1 after cycling.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
A preparation method of a lithium titanate electrode for inhibiting gas generation comprises the following steps:
(1) 0.3L of mixed solution of ammonium dihydrogen phosphate and ammonium fluoride with the concentration of 0.02mol/L is prepared;
(2) adding 7.2g of lithium titanate into the mixed solution in the step (1), and fully stirring to form a suspension;
(3) slowly dripping 0.5L of lithium hydroxide solution with the concentration of 0.04mol/L into the suspension liquid in the step (2) at the dripping speed of 0.5mL/min, fully stirring, and filtering to obtain filter residue;
(4) repeatedly washing the filter residue obtained in the step (3) with deionized water until the existence of ammonium ions and lithium ions cannot be detected in the washing liquid;
(5) drying the product obtained in the step (4), and fully grinding;
(6) and (4) carrying out heat treatment on the product obtained in the step (5) at 400 ℃ in a nitrogen atmosphere for 2h to obtain the lithium titanate electrode coated by the lithium fluoride and the lithium phosphate. The lithium titanate electrode comprises 3% of lithium phosphate and 3% of lithium fluoride by mass; the mass ratio of lithium phosphate to lithium fluoride is 1.12: 1.
example 2
A preparation method of a lithium titanate electrode for inhibiting gas generation comprises the following steps:
(1) 0.1L of mixed solution of ammonium dihydrogen phosphate and ammonium fluoride with the concentration of 0.08mol/L is prepared;
(2) adding 10.4g of lithium titanate into the mixed solution in the step (1), and fully stirring to form a suspension;
(3) slowly dripping 0.5L of lithium hydroxide solution with the concentration of 0.04mol/L into the suspension liquid in the step (2) at the dripping speed of 0.2mL/min, fully stirring, and filtering to obtain filter residue;
(4) repeatedly washing the filter residue obtained in the step (3) with deionized water until the existence of ammonium ions and lithium ions cannot be detected in the washing liquid;
(5) drying the product obtained in the step (4), and fully grinding;
(6) and (4) carrying out heat treatment on the product obtained in the step (5) at the temperature of 300 ℃ in a nitrogen atmosphere for 4h to obtain the lithium titanate electrode coated by the lithium fluoride and the lithium phosphate. The lithium titanate electrode comprises 2.62% of lithium phosphate and lithium fluoride by mass; the mass ratio of the lithium phosphate to the lithium fluoride is 1: 2.
example 3
A preparation method of a lithium titanate electrode for inhibiting gas generation comprises the following steps:
(1) 0.2L of mixed solution of ammonium dihydrogen phosphate and ammonium fluoride with the concentration of 0.04mol/L is prepared;
(2) adding 19g of lithium titanate into the mixed solution obtained in the step (1), and fully stirring to form a suspension;
(3) slowly dripping 0.5L of lithium hydroxide solution with the concentration of 0.2mol/L into the suspension liquid in the step (2) at the dripping speed of 1mL/min, fully stirring, and filtering to obtain filter residue;
(4) repeatedly washing the filter residue obtained in the step (3) with deionized water until the existence of ammonium ions and lithium ions cannot be detected in the washing liquid;
(5) drying the product obtained in the step (4), and fully grinding;
(6) and (4) carrying out heat treatment on the product obtained in the step (5) at 600 ℃ in a nitrogen atmosphere for 3h to obtain the lithium titanate electrode coated by the lithium fluoride and the lithium phosphate. The lithium titanate electrode comprises 2% of lithium phosphate and lithium fluoride by mass; the mass ratio of the lithium phosphate to the lithium fluoride is 1.5: 1.
the electrochemical performance test method is characterized in that lithium titanate coated by lithium fluoride and lithium phosphate is used as a negative electrode, and the electrochemical performance test method comprises the following specific steps:
assembling the soft package battery: an 2645110 type soft package battery with the thickness of 2.6mm, the width of 45mm and the length of 110mm is adopted, nickel lithium manganate is taken as a positive electrode, lithium fluoride and lithium phosphate co-coated lithium titanate in example 1 are taken as a negative electrode, the capacity is designed to be 3300mAh, Celgard2400 is taken as a diaphragm, and 1mol/L LiPF6DEC and DMC (volume ratio 1:1:1) are used as electrolyte, and gas production is observed at 1.2-2.8V, normal temperature, 0.2C charge/0.5C discharge and 300 times of circulation.
Comparative example 1
The method comprises the following specific steps of using lithium titanate without being coated as a negative electrode, and testing electrochemical performance:
assembling the soft package battery: an 2645110 type soft package battery with the thickness of 2.6mm, the width of 45mm and the length of 110mm is adopted, nickel lithium manganate is taken as a positive electrode, lithium titanate is taken as a negative electrode, the capacity is designed to be 3300mAh, Celgard2400 is taken as a diaphragm, and 1mol/L LiPF6DEC and DMC (volume ratio 1:1:1) are used as electrolyte, and gas production is observed at 1.2-2.8V, normal temperature, 0.2C charge/0.5C discharge and 300 times of circulation.
Characterization results of lithium titanate electrodes co-coated with lithium fluoride and lithium phosphate in example 1 of the present invention and uncoated lithium titanate electrodes in comparative example 1 are: as can be seen from fig. 1, a significant coating can be observed on the surface of lithium titanate co-coated with lithium fluoride and lithium phosphate, while the uncoated lithium titanate of fig. 2 has a smooth surface and no attachment; fig. 3 shows that the swelling and swelling of the soft-package battery composed of lithium titanate which is not coated can be observed, and the swelling of the soft-package battery composed of lithium titanate which is coated by lithium fluoride and lithium phosphate is not observed; as can be seen from a comparison between fig. 4 and fig. 5, after an electrochemical test, the lithium titanate electrode co-coated with lithium fluoride and lithium phosphate generates less irregular impurities on the surface of the electrode, that is, fewer electrolyte decomposition products, while the uncoated lithium titanate electrode generates a large amount of irregular fragments, that is, more electrolyte decomposition products, indicating that the electrode material modified by coating has less catalytic decomposition on the electrolyte, and the lithium fluoride and lithium phosphate co-coated modified lithium titanate can effectively inhibit the lithium titanate electrode from swelling and generating gas.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A lithium titanate electrode for suppressing gas evolution, characterized in that the electrode is composed of lithium titanate and lithium phosphate and lithium fluoride closely adhered to the surface thereof.
2. The lithium titanate electrode for suppressing gas evolution as claimed in claim 1, wherein the size of lithium titanate in the electrode is 100nm to 1 μm.
3. The lithium titanate electrode for inhibiting gas evolution as claimed in claim 1, wherein the lithium phosphate and the lithium fluoride are mixed together and coated on the surface of the lithium titanate.
4. The lithium titanate electrode capable of inhibiting gas evolution as claimed in claim 1 or 3, wherein the lithium phosphate and the lithium fluoride account for 0.1-3% of the lithium titanate electrode by mass.
5. The gas evolution-inhibiting lithium titanate electrode according to claim 1 or 3, wherein the mass ratio of lithium phosphate to lithium fluoride in the lithium titanate electrode is 1: 10-10: 1.
6. a method for preparing a gas evolution-inhibiting lithium titanate electrode according to claim 1, comprising the steps of:
(1) dissolving ammonium dihydrogen phosphate and ammonium fluoride in deionized water to form a mixed solution with the concentration of 0.01-0.1 mol/L;
(2) adding lithium titanate into the mixed solution obtained in the step (1), and fully stirring to form a suspension;
(3) slowly dripping 0.04mol/L-0.4mol/L lithium hydroxide solution into the suspension obtained in the step (2), fully stirring, and filtering to obtain filter residue;
(4) repeatedly washing the filter residue obtained in the step (3) with deionized water until the existence of ammonium ions and lithium ions cannot be detected in the washing liquid;
(5) drying the product obtained in the step (4), and fully grinding;
(6) and (4) carrying out heat treatment on the product obtained in the step (5) in an inert atmosphere at the temperature of 300-600 ℃ for 2-6h to obtain the lithium titanate electrode which is coated by the lithium fluoride and the lithium phosphate.
7. The method for preparing a lithium titanate electrode capable of inhibiting gas evolution according to claim 6, wherein in the step (3), the dropping speed of the lithium hydroxide solution is 0.1-1 mL/min.
8. The method for preparing a lithium titanate electrode capable of inhibiting gas evolution according to claim 6, wherein in the step (6), the heat treatment temperature is 400 ℃ and the heat treatment time is 2 hours.
9. The method for preparing a lithium titanate electrode capable of inhibiting gassing according to claim 6 wherein in step (6) the inert atmosphere of the heat treatment is nitrogen or argon.
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- 2020-12-23 CN CN202011538469.2A patent/CN112670446A/en active Pending
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Application publication date: 20210416 |