CN105552356A - Preparation method of wide-potential window anode material for lithium-ion battery - Google Patents

Preparation method of wide-potential window anode material for lithium-ion battery Download PDF

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Publication number
CN105552356A
CN105552356A CN201511005962.7A CN201511005962A CN105552356A CN 105552356 A CN105552356 A CN 105552356A CN 201511005962 A CN201511005962 A CN 201511005962A CN 105552356 A CN105552356 A CN 105552356A
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lithium
ion battery
potential window
source
preparation
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CN105552356B (en
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伊廷锋
梅洁
朱彦荣
诸荣孙
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Anhui University of Technology AHUT
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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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • 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
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a preparation method of a wide-potential window anode material for a lithium-ion battery, and belongs to the technical field of lithium-ion batteries. A chemical formula of the material is Li5Cr9Ti4O24-aCr2O3, wherein a is smaller than or equal to 0.2 and greater than or equal to 0.05. The material is prepared through a triethanolamine-assisted sol-gel method. The anode material has sub-micron particle sizes, good dispersity, high crystallinity, considerable wide-potential window reversible capacity, excellent rate capability, stable cycle lifetime, relatively high theoretical capacity and rapid charge and discharge performance; the energy density and the power density of the lithium-ion battery are improved; and the usage amount of a lithium element is reduced, so that the cost is reduced; and the preparation method can be applied to the high-performance anode material for the lithium-ion battery.

Description

A kind of preparation method of lithium ion battery negative material of broad potential window
Technical field
The invention belongs to technical field of lithium ion, be specifically related to the preparation method of the lithium ion battery negative material of broad potential window.
Background technology
Along with the development of various electronic equipment and electric automobile, hybrid vehicle, have higher requirement to providing the lithium ion battery of energy for it.Capacity density and the energy density of lithium ion battery are higher, are acknowledged as most promising electrokinetic cell.Current commercial li-ion cell negative electrode material adopts various embedding lithium carbon/graphite material mostly, but, the intercalation potential (0 ~ 0.26V) of material with carbon element is very close with the sedimentation potential of lithium metal, when over-charging of battery, lithium metal may be separated out in carbon electrodes and form Li dendrite, dendrite further growth, then may pierce through barrier film, cause both positive and negative polarity to connect, thus cause short circuit; In addition, material with carbon element also exist first charge-discharge efficiency low, have an effect, there is the shortcomings such as obvious voltage delay phenomenon, preparation method's more complicated with electrolyte.Spinel type lithium titanate Li 4ti 5o 12be a kind of " zero strain " material, in the process that Lithium-ion embeding is deviate from, crystal structure can keep the stability of height, and makes it have excellent cycle performance and stable discharge voltage.And there is relatively high electrode voltage (1.55V), in whole discharge process, there will not be the precipitation of lithium metal, substantially increase the fail safe that electrode material uses.But Li 4ti 5o 12maximum deficiency is that its electronic conductance and ionic conductance are lower, thus when high current charge-discharge, capacity attenuation is fast, high rate performance is poor.Li 4ti 5o 12/ Li half-cell discharge is to (vs.Li during 0V +/ Li), theoretical capacity is 293mAh/g, and reversible capacity can not reach required target call.Therefore, the titanate negative material of necessary development of new is had very much.Li 5cr 9ti 4o 24as a kind of novel titanate negative material, (vs.Li when being discharged to 0V +/ Li), theoretical capacity is 323mAh/g.Although there is report (ChunfuLinetal.JournalofAlloysandCompounds, 2015, the 650:616-621.) Li that adopted high temperature solid-state method to prepare before this 5cr 9ti 4o 24negative material, but the usual particle diameter of material prepared by high temperature solid-state method is larger, uneven, energy consumption is high.In addition, consider that electrokinetic cell often there will be abuse or overdischarge behavior, research Li 5cr 9ti 4o 24fail safe during negative material overdischarge seems particularly important, i.e. broad potential window performance.
Summary of the invention
For overcoming prior art Problems existing, the object of this invention is to provide one and preparing Li 5cr 9ti 4o 24-Cr 2o 3the method of composite negative pole material, to obtaining the broad potential window negative material with fast charging and discharging characteristic and high cyclical stability.
Preparation method's concrete steps of the lithium ion battery negative material of broad potential window provided by the present invention are as follows:
Titanium source and chromic nitrate are dissolved in ethanol solution, triethanolamine is added under the condition stirred, and then the ethanol water added containing lithium source, then in 70 DEG C of water-baths, gel is heated with stirring to, then 80-100 DEG C of oven dry in an oven, pre-burning 6-8h at 500-600 DEG C is put in Muffle furnace after grinding, be cooled to room temperature, ball milling 3-4h in ball mill, sieve, put into Muffle furnace again and burn 10-15h at 750-900 DEG C, be cooled to room temperature, be i.e. the lithium ion battery negative material Li of obtained broad potential window 5cr 9ti 4o 24-aCr 2o 3, wherein 0.05≤a≤0.2.
The mol ratio in described titanium source, chromic nitrate, triethanolamine and lithium source is 1:2.275 ~ 2.35:3.5 ~ 5:1.25.
Described lithium source is the one in lithium acetate, lithium nitrate, lithium hydroxide; Described titanium source is the one in butyl titanate, metatitanic acid orthocarbonate.
As one optimization, the mol ratio in described titanium source, chromic nitrate, triethanolamine and lithium source is 1:2.3:4.5:1.25; Described lithium source is lithium acetate; Described titanium source is butyl titanate.
The chemical formula of the lithium ion battery negative material of the broad potential window prepared by the present invention is: Li 5cr 9ti 4o 24-aCr 2o 3, wherein 0.05≤a≤0.2, this negative material is the particle diameter having submicron order, has good chemical property, can be used for high performance lithium ionic cell cathode material.
Compared with prior art, the present invention has following technique effect:
(1) Li prepared 5cr 9ti 4o 24-Cr 2o 3composite negative pole material controllability is good, and reappearance is high.
(2) the material granule uniformity utilizing the method to synthesize, good dispersion, degree of crystallinity are high, and the material obtained is the particle diameter of submicron order, are conducive to the chemical property improving material.
(3) material obtained in the present invention has considerable broad potential window reversible capacity, excellent high rate performance and stable cycle life, make this material have very high actual use value, effectively can meet the actual requirement of the various application of lithium ion battery.
(4) the present invention develops lithium ion battery negative material and has higher theoretical capacity and charge-discharge performance fast, improves energy density and the power density of lithium ion battery, use raw material cheap and easy to get.
(5) present invention reduces the use amount of elemental lithium, thus reduce cost.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 gained Li 5cr 9ti 4o 24-0.1Cr 2o 3xRD figure.
Fig. 2 is the embodiment of the present invention 1 gained Li 5cr 9ti 4o 24-0.1Cr 2o 3sEM figure.
Fig. 3 is the embodiment of the present invention 1 gained Li 5cr 9ti 4o 24-0.1Cr 2o 3fT-IR figure.
Fig. 4 is the embodiment of the present invention 1 gained Li 5cr 9ti 4o 24-0.1Cr 2o 3first charge-discharge curve.
Fig. 5 is the embodiment of the present invention 1 gained Li 5cr 9ti 4o 24-0.1Cr 2o 310C circulation performance curve.
Embodiment
Below in conjunction with specific embodiment in detail the present invention is described in detail, but the present invention is not limited to following embodiment.
Embodiment 1
By the butyl titanate (C of 0.04mol 16h 36o 4and 0.092mol chromic nitrate Cr (NO Ti) 3) 39H 2o is dissolved in ethanol solution, adds 0.18molTEA (triethanolamine), and then add containing 0.05mol lithium acetate (CH under the condition stirred 3cOOLi2H 2o) ethanol water (containing 20mL ethanol and 30mL water) solution, then in 70 DEG C of water-baths, gel is heated with stirring to, then 100 DEG C of oven dry in an oven, to be put in Muffle furnace pre-burning 8h at 500 DEG C after grinding, to be cooled to room temperature, ball milling 3h in ball mill, sieve, put into Muffle furnace again and burn 12h at 800 DEG C, be cooled to room temperature, be i.e. the lithium ion battery negative material Li of obtained broad potential window 5cr 9ti 4o 24-0.1Cr 2o 3.X-ray powder diffraction and infrared spectrum analysis show that the product obtained of gained is Li 5cr 9ti 4o 24-0.1Cr 2o 3compound, degree of crystallinity high (as shown in figures 1 and 3).Learn that the even particle size of products therefrom is consistent from scanning electron microscope analysis, particle diameter is 200-500nm (as shown in Figure 2).Using the product of gained as electrode material, in the glove box being full of argon gas, be assembled into experiment fastening lithium ionic cell, between 0-2.5V, carry out charge and discharge cycles with the multiplying power of 0.2C, Li 5cr 9ti 4o 24-Cr 2o 3discharge capacity is 357.2mAhg first -1(as shown in Figure 4).10C multiplying power first discharge capacity is 111.8mAhg -1, the reversible capacity after circulating 200 weeks is 85.5mAhg -1, Li 5cr 9ti 4o 24-0.1Cr 2o 3show excellent broad potential window fast charging and discharging performance (as shown in Figure 5).
Embodiment 2
By the butyl titanate (C of 0.04mol 16h 36o 4and 0.092mol chromic nitrate Cr (NO Ti) 3) 39H 2o is dissolved in ethanol solution, 0.18molTEA (triethanolamine) is added under the condition stirred, and then ethanol water (containing 20mL ethanol and the 30mL water) solution added containing 0.05mol lithium hydroxide, then in 70 DEG C of water-baths, gel is heated with stirring to, then 80 DEG C of oven dry in an oven, pre-burning 8h at 600 DEG C is put in Muffle furnace after grinding, be cooled to room temperature, ball milling 4h in ball mill, sieve, put into Muffle furnace again and burn 15h at 900 DEG C, be cooled to room temperature, be i.e. the lithium ion battery negative material Li of obtained broad potential window 5cr 9ti 4o 24-0.1Cr 2o 3.X-ray powder diffraction and infrared spectrum analysis show that the product obtained of gained is Li 5cr 9ti 4o 24-0.1Cr 2o 3compound, degree of crystallinity is high.Learn that the even particle size of products therefrom is consistent from scanning electron microscope analysis, particle diameter is 200-500nm.Using the product of gained as electrode material, in the glove box being full of argon gas, be assembled into experiment fastening lithium ionic cell, between 0-2.5V, carry out charge and discharge cycles with the multiplying power of 0.2C, Li 5cr 9ti 4o 24-Cr 2o 3discharge capacity is 351.2mAhg first -1.10C multiplying power first discharge capacity is 110.6mAhg -1, the reversible capacity after circulating 200 weeks is 82.6mAhg -1, Li 5cr 9ti 4o 24-0.1Cr 2o 3show excellent broad potential window fast charging and discharging performance.
Embodiment 3
By the butyl titanate (C of 0.04mol 16h 36o 4and 0.091mol chromic nitrate Cr (NO Ti) 3) 39H 2o is dissolved in ethanol solution, 0.15molTEA (triethanolamine) is added under the condition stirred, and then ethanol water (containing 20mL ethanol and the 30mL water) solution added containing 0.05mol lithium hydroxide, then in 70 DEG C of water-baths, gel is heated with stirring to, then 80 DEG C of oven dry in an oven, pre-burning 8h at 600 DEG C is put in Muffle furnace after grinding, be cooled to room temperature, ball milling 4h in ball mill, sieve, put into Muffle furnace again and burn 15h at 900 DEG C, be cooled to room temperature, be i.e. the lithium ion battery negative material Li of obtained broad potential window 5cr 9ti 4o 24-0.05Cr 2o 3.X-ray powder diffraction and infrared spectrum analysis show that the product obtained of gained is Li 5cr 9ti 4o 24-0.05Cr 2o 3compound, degree of crystallinity is high.Learn that the even particle size of products therefrom is consistent from scanning electron microscope analysis, particle diameter is 200-600nm.Using the product of gained as electrode material, in the glove box being full of argon gas, be assembled into experiment fastening lithium ionic cell, between 0-2.5V, carry out charge and discharge cycles with the multiplying power of 0.2C, Li 5cr 9ti 4o 24-Cr 2o 3discharge capacity is 301.4mAhg first -1.10C multiplying power first discharge capacity is 109.5mAhg -1, the reversible capacity after circulating 200 weeks is 80.3mAhg -1, Li 5cr 9ti 4o 24-0.05Cr 2o 3show excellent broad potential window fast charging and discharging performance.
Embodiment 4
By the butyl titanate (C of 0.04mol 16h 36o 4and 0.094mol chromic nitrate Cr (NO Ti) 3) 39H 2o is dissolved in ethanol solution, adds 0.2molTEA (triethanolamine), and then add containing 0.05mol lithium acetate (CH under the condition stirred 3cOOLi2H 2o) ethanol water (containing 20mL ethanol and 30mL water) solution, then in 70 DEG C of water-baths, gel is heated with stirring to, then 100 DEG C of oven dry in an oven, to be put in Muffle furnace pre-burning 8h at 500 DEG C after grinding, to be cooled to room temperature, ball milling 3h in ball mill, sieve, put into Muffle furnace again and burn 12h at 800 DEG C, be cooled to room temperature, be i.e. the lithium ion battery negative material Li of obtained broad potential window 5cr 9ti 4o 24-0.2Cr 2o 3.X-ray powder diffraction and infrared spectrum analysis show that the product obtained of gained is Li 5cr 9ti 4o 24-0.2Cr 2o 3compound, degree of crystallinity is high.Learn that the even particle size of products therefrom is consistent from scanning electron microscope analysis, particle diameter is 200-500nm.Using the product of gained as electrode material, in the glove box being full of argon gas, be assembled into experiment fastening lithium ionic cell, between 0-2.5V, carry out charge and discharge cycles with the multiplying power of 0.2C, Li 5cr 9ti 4o 24-0.2Cr 2o 3discharge capacity is 359.5mAhg first -1.10C multiplying power first discharge capacity is 110.9mAhg -1, the reversible capacity after circulating 200 weeks is 84.7mAhg -1, Li 5cr 9ti 4o 24-0.2Cr 2o 3show excellent broad potential window fast charging and discharging performance.
Embodiment 5
By the metatitanic acid orthocarbonate of 0.04mol and 0.091mol chromic nitrate Cr (NO 3) 39H 2o is dissolved in ethanol solution, 0.14molTEA (triethanolamine) is added under the condition stirred, and then ethanol water (containing 20mL ethanol and the 30mL water) solution added containing 0.05mol lithium nitrate, then in 70 DEG C of water-baths, gel is heated with stirring to, then 80 DEG C of oven dry in an oven, pre-burning 6h at 500 DEG C is put in Muffle furnace after grinding, be cooled to room temperature, ball milling 4h in ball mill, sieve, put into Muffle furnace again and burn 15h at 750 DEG C, be cooled to room temperature, be i.e. the lithium ion battery negative material Li of obtained broad potential window 5cr 9ti 4o 24-0.05Cr 2o 3.X-ray powder diffraction and infrared spectrum analysis show that the product obtained of gained is Li 5cr 9ti 4o 24-0.05Cr 2o 3compound, degree of crystallinity is high.Learn that the even particle size of products therefrom is consistent from scanning electron microscope analysis, particle diameter is 200-600nm.Using the product of gained as electrode material, in the glove box being full of argon gas, be assembled into experiment fastening lithium ionic cell, between 0-2.5V, carry out charge and discharge cycles with the multiplying power of 0.2C, Li 5cr 9ti 4o 24-Cr 2o 3discharge capacity is 297.1mAhg first -1.10C multiplying power first discharge capacity is 109.3mAhg -1, the reversible capacity after circulating 200 weeks is 80mAhg -1, Li 5cr 9ti 4o 24-0.05Cr 2o 3show excellent broad potential window fast charging and discharging performance.
Embodiment 6
By the metatitanic acid orthocarbonate of 0.04mol and 0.094mol chromic nitrate Cr (NO 3) 39H 2o is dissolved in ethanol solution, 0.19molTEA (triethanolamine) is added under the condition stirred, and then ethanol water (containing 20mL ethanol and the 30mL water) solution added containing 0.05mol lithium nitrate, then in 70 DEG C of water-baths, gel is heated with stirring to, then 100 DEG C of oven dry in an oven, pre-burning 8h at 600 DEG C is put in Muffle furnace after grinding, be cooled to room temperature, ball milling 4h in ball mill, sieve, put into Muffle furnace again and burn 15h at 900 DEG C, be cooled to room temperature, be i.e. the lithium ion battery negative material Li of obtained broad potential window 5cr 9ti 4o 24-0.2Cr 2o 3.X-ray powder diffraction and infrared spectrum analysis show that the product obtained of gained is Li 5cr 9ti 4o 24-0.2Cr 2o 3compound, degree of crystallinity is high.Learn that the even particle size of products therefrom is consistent from scanning electron microscope analysis, particle diameter is 200-700nm.Using the product of gained as electrode material, in the glove box being full of argon gas, be assembled into experiment fastening lithium ionic cell, between 0-2.5V, carry out charge and discharge cycles with the multiplying power of 0.2C, Li 5cr 9ti 4o 24-0.2Cr 2o 3discharge capacity is 355.6mAhg first -1.10C multiplying power first discharge capacity is 108.5mAhg -1, the reversible capacity after circulating 200 weeks is 84.1mAhg -1, Li 5cr 9ti 4o 24-0.2Cr 2o 3show excellent broad potential window fast charging and discharging performance.

Claims (2)

1. a preparation method for the lithium ion battery negative material of broad potential window, is characterized in that, the concrete steps of the method are as follows:
Titanium source and chromic nitrate are dissolved in ethanol solution, triethanolamine is added under the condition stirred, and then the ethanol water added containing lithium source, then in 70 DEG C of water-baths, gel is heated with stirring to, then 80-100 DEG C of oven dry in an oven, pre-burning 6-8h at 500-600 DEG C is put in Muffle furnace after grinding, be cooled to room temperature, ball milling 3-4h in ball mill, sieve, put into Muffle furnace again and burn 10-15h at 750-900 DEG C, be cooled to room temperature, be i.e. the lithium ion battery negative material Li of obtained broad potential window 5cr 9ti 4o 24-aCr 2o 3, wherein 0.05≤a≤0.2;
The mol ratio in described titanium source, chromic nitrate, triethanolamine and lithium source is 1:2.275 ~ 2.35:3.5 ~ 5:1.25;
Described lithium source is the one in lithium acetate, lithium nitrate, lithium hydroxide; Described titanium source is the one in butyl titanate, metatitanic acid orthocarbonate.
2. the preparation method of the lithium ion battery negative material of a kind of broad potential window as claimed in claim 1, is characterized in that, the mol ratio in described titanium source, chromic nitrate, triethanolamine and lithium source is 1:2.3:4.5:1.25; Described lithium source is lithium acetate; Described titanium source is butyl titanate.
CN201511005962.7A 2015-12-28 2015-12-28 A kind of preparation method of the lithium ion battery negative material of broad potential window Active CN105552356B (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN105932272A (en) * 2016-05-23 2016-09-07 渤海大学 Preparation method of chromium lithium titanate nano-material
CN110176584A (en) * 2019-05-14 2019-08-27 南京国轩电池有限公司 A kind of preparation method of lithium ion battery titanate composite negative pole material
CN115595564A (en) * 2022-10-18 2023-01-13 华中科技大学（Cn） Novel Cr 2 O 3 Coating and method for producing the same

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105932272A (en) * 2016-05-23 2016-09-07 渤海大学 Preparation method of chromium lithium titanate nano-material
CN105932272B (en) * 2016-05-23 2018-11-13 渤海大学 A kind of preparation method of metatitanic acid chromium lithium nano material
CN110176584A (en) * 2019-05-14 2019-08-27 南京国轩电池有限公司 A kind of preparation method of lithium ion battery titanate composite negative pole material
CN110176584B (en) * 2019-05-14 2022-09-06 南京国轩电池有限公司 Preparation method of titanate composite negative electrode material for lithium ion battery
CN115595564A (en) * 2022-10-18 2023-01-13 华中科技大学（Cn） Novel Cr 2 O 3 Coating and method for producing the same

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