CN103594694A - Preparation method of spherical lithium titanate ion battery cathode material - Google Patents

Preparation method of spherical lithium titanate ion battery cathode material Download PDF

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CN103594694A
CN103594694A CN201310615695.XA CN201310615695A CN103594694A CN 103594694 A CN103594694 A CN 103594694A CN 201310615695 A CN201310615695 A CN 201310615695A CN 103594694 A CN103594694 A CN 103594694A
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ion battery
titanium dioxide
lithium
lithium titanate
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刁国旺
陈铭
李伟
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Yangzhou University
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C01G23/005—Alkali titanates
    • 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 relates to a preparation method of a spherical lithium titanate ion battery cathode material, which belongs to the lithium ion battery energy material technical field, the method comprises the following steps: uniformly mixing absolute ethyl alcohol and a potassium chloride aqueous solution, adding tetrabutyl titanate drop by drop, uniformly mixing, standing at normal temperature, centrifuging after completing the reaction, taking a solid phase for washing, drying to obtain titanium dioxide ball, uniformly dispersing an aqueous solution of soluble lithium salt and titanium dioxide ball in ultrasound and then performing a hydro-thermal reaction, centrifuging after completing the reaction, taking the solid phase for washing, and drying and calcining to obtain spherical lithium titanate ion battery cathode material. The preparation method has the advantages of simple process and high yield, the obtained lithium titanate ion battery cathode material has the advantages of uniform morphology and good crystallization degree, a porous structure is provided in the inner part, the spherical lithium titanate belongs to the spinel type, and can replace a carbon material to become the lithium ion battery cathode material.

Description

A kind of preparation method of spherical metatitanic acid lithium ion battery negative material
Technical field
The invention belongs to lithium-ion battery energy material technology field, be specifically related to prepare the method for spherical lithium titanate lithium ion battery negative material.
Background technology
Mankind's modern life more and more be unable to do without movably chemical power source, wherein, lithium rechargeable battery has extended cycle life with it, specific capacity is large, the many advantages successes such as memory-less effect and operating voltage are high are also widely used in mobile phone, video camera, in all kinds of Miniature Portable Units such as laptop computer, meanwhile, although various lithium ion battery negative materials still be take various graphite type material as main at present, but other various negative materials have also obtained development rapidly aspect basic research, as tin-based material, silica-base material, metal oxide materials nitride material and lithium titanate material etc.
With carbon negative electrode lithium ion storage battery, be widely used.But it also existent defect, as very approaching in the current potential of the current potential of carbon negative pole and lithium, during over-charging of battery, lithium metal may be separated out and cause safety problem in carbon electrodes; The speed releasing energy is fast not, is not suitable for equipment needing moment heavy current etc.And lithium titanate has " zero strain " characteristic that in charge and discharge process, skeleton structure changes hardly, embedding lithium current potential high and be difficult for causing that lithium metal is separated out, coulombic efficiency is high, lithium ion diffusion coefficient is than good characteristics such as the high orders of magnitude of carbon negative pole, possessed the characteristic that the essential charging times of lithium-ions battery of future generation is more, charging process is faster, safer.If the negative material using lithium titanate as lithium-ions battery, is sacrificing under the prerequisite of certain specific energy, can improve fast charging and discharging performance, circulation and the security performance of system.But lithium titanate also has its deficiency, as high potential brings the low-voltage of battery, poorly conductive, heavy-current discharge easily produces larger polarization etc., therefore, need to carry out modification to material, as by mixing metal ion, by carbon, be coated all means and improve its conductivity, improve electron conduction and chemical property, large multiplying power discharging capacity and cyclical stability are also improved significantly, or pass through nanometer, reduce its size, make it there is nano effect, improve its chemical property, as Jizhang Chen prepares jagged lithium titanate, this material is under high magnification electric current, it is good that cycle performance still keeps, (Jizhang Chen .Synthesis of sawtooth ~ like Li 4ti 5o 12nanosheets as anode materials for Li ~ ion batteries .[J] Electrochimica Acta 55 (2010) 6596 – 6600) so, by changing lithium titanate pattern, can change its chemical property.
Summary of the invention
The object of the invention is to propose a kind of spherical lithium titanate (Li that has both lithium ion carbon negative electrode lithium ion battery advantage 4ti 5o 12) preparation method of lithium ion battery negative material.
This bright technical scheme comprises the following steps:
1) after absolute ethyl alcohol is mixed with potassium chloride solution, then drip butyl titanate, then after mixing, standing reaction at normal temperatures, question response finishes rear centrifugal, gets solid phase washing, dries, and obtains titanium dioxide ball;
2) carry out hydro-thermal reaction after the aqueous solution of solubility lithium salts and titanium dioxide ball are uniformly dispersed in ultrasonic, question response finishes rear centrifugal, gets solid phase washing, dries, and then calcining, obtains spherical metatitanic acid lithium ion battery negative material.
Preparation method of the present invention is easy, easy to operate, and cost is low, nonhazardous, and productive rate is high, and reactant ethanol can also reclaim and reuse in addition.
The spherical metatitanic acid lithium ion battery negative material pattern homogeneous that the present invention obtains, diameter is 300nm～500nm, better crystallinity degree, there is loose structure inside, this structure can reduce the diffusion length of lithium ion, thereby improves greatly the diffusion rate of lithium ion in material, can improve the performance of lithium ion battery, this spherical lithium titanate is to belong to spinel-type, can replace material with carbon element as lithium ion battery negative material.The complicated spherical pattern of geometry makes it have larger specific area, can store more lithium ions, improves the lithium storage content of lithium titanate.
In addition, the concentration of potassium chloride solution of the present invention is 0.1mol/L.This concentration can well be dispersed in ethanolic solution, and as a kind of spherical template agent concentration, this concentration is optimal.
The volume ratio that feeds intake of described absolute ethyl alcohol, potassium chloride solution and butyl titanate is 100～200 ︰ 0.2～1 ︰ 2～3.Within the scope of this volume ratio, tetrabutyl titanate hydrolysis speed is suitable, and hydrolysis completely, can form the uniform titanium dioxide ball of pattern.
Described solubility lithium salts is LiOH.H 2o, Li 2cO 3or LiCl.Solubility lithium salts is to provide lithium source, LiOHH for product lithium titanate 2o, Li 2cO 3strong basicity can promote reaction, be to react completely, and the neutrality of LiCl, reaction effect is such as two kinds above.
The concentration of the aqueous solution of solubility lithium salts is 0.2 mol/L～1mol/L.In this proportion, solution is more easily prepared, and uses maximum.
The mass ratio of described solubility lithium salts and titanium dioxide ball is 25～1 ︰ 1.This quality, than in scope, is the crucial mass ratio that synthesizes spinel type lithium titanate, and the lithium titanate product purity synthesizing is high, pattern homogeneous, good dispersion degree.
The condition of described ultrasonic processing is: 50～55KHz, and under this ultrasound condition, reactant can be dispersed in solvent uniformly, and fully contact, reacts completely.
The temperature conditions of described hydro-thermal reaction is 100 ℃～200 ℃, and the time is 2h～24h.In this temperature and time scope, reactant can fully activate under hydrothermal condition, reacts completely, and generating gradually pattern is spherical lithium titanate.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the titanium dioxide ball that under normal temperature, sol-gel reaction was taken after 24 hours.
The SEM figure that Fig. 2 is the product of shooting react 15 hours under 180 ℃ of hydrothermal conditions after.
Fig. 3 is the XRD figure of 800 ℃ of calcining afterproducts react 15 hours under 180 ℃ of hydrothermal conditions after.
Fig. 4 is the cyclic voltammetry curve figure that product is assembled into rear button cell test.
Fig. 5 is the charge-discharge performance figure that product is assembled into rear button cell test.
Embodiment
One, below in conjunction with embodiment, the present invention is described in detail:
embodiment 1
Figure 201310615695X100002DEST_PATH_IMAGE001
prepare titanium dioxide ball: the solution that adds the 0.1mol/L potassium chloride of 0.2ml in the absolute ethyl alcohol of 100ml, after stirring with mechanical agitator, drip butyl titanate 2ml, after mechanical agitation 1h, at room temperature standing 24h reacts, reaction finishes rear centrifugal, gets solid phase through washing, oven dry, is titanium dioxide ball.Liquid phase is carried out Distillation recovery, obtains ethanol recycling.
Figure 492758DEST_PATH_IMAGE002
prepare spherical metatitanic acid lithium ion battery negative material: getting concentration is 0.2 mol/L solubility lithium salt solution 20ml, then add 0.1g titanium dioxide ball, ultrasonic dispersion is after 25 minutes, be placed in 100 ℃ of Water Under thermal response 2h, after reaction finishes, product is centrifugal, get solid phase, adopt deionized water and absolute ethyl alcohol to wash respectively three times, after then drying, be placed in again at 500 ℃ and calcine 1～5h.End product is spherical metatitanic acid lithium ion battery negative material.
embodiment 2
Figure 423805DEST_PATH_IMAGE001
prepare titanium dioxide ball: the solution of the 0.1mol/L potassium chloride of 1ml will be added in the absolute ethyl alcohol of 200ml, after stirring with mechanical agitator, drip butyl titanate 3ml, after mechanical agitation 1h, at room temperature standing 24h reacts, reaction finishes rear centrifugal, gets solid phase through washing, oven dry, is titanium dioxide ball.Liquid phase is carried out Distillation recovery, obtains ethanol recycling.
Figure 178135DEST_PATH_IMAGE002
prepare spherical metatitanic acid lithium ion battery negative material: getting concentration is that then 1 mol/L solubility lithium salt solution 50ml adds 0.5g titanium dioxide ball, ultrasonic dispersion is after 25 minutes, be placed in 200 ℃ of Water Under thermal response 24h, after reaction finishes, product is centrifugal, get solid phase, adopt deionized water and absolute ethyl alcohol to wash respectively three times, after then drying, be placed in again at 700 ℃ and calcine 2h.End product is spherical metatitanic acid lithium ion battery negative material.
embodiment 3
prepare titanium dioxide ball: the solution of the 0.1mol/L potassium chloride of 0.3l will be added in the absolute ethyl alcohol of 150ml, after stirring with mechanical agitator, drip butyl titanate 2.5ml, after mechanical agitation 1h, at room temperature standing 24h reacts, reaction finishes rear centrifugal, gets solid phase through washing, oven dry, is titanium dioxide ball.Liquid phase is carried out Distillation recovery, obtains ethanol recycling.
prepare spherical metatitanic acid lithium ion battery negative material: getting concentration is that then 0.3mol/L solubility lithium salt solution 30ml adds 0.5g titanium dioxide ball, ultrasonic dispersion is after 25 minutes, be placed in 150 ℃ of Water Under thermal response 8h, after reaction finishes, product is centrifugal, get solid phase, adopt deionized water and absolute ethyl alcohol to wash respectively three times, after then drying, be placed in again at 600 ℃ and calcine 2h.End product is spherical metatitanic acid lithium ion battery negative material.
embodiment 4
Figure 55327DEST_PATH_IMAGE001
prepare titanium dioxide ball: the solution of the 0.1mol/L potassium chloride of 0.7ml will be added in the absolute ethyl alcohol of 150ml, after stirring with mechanical agitator, drip butyl titanate 2.7ml, after mechanical agitation 1h, at room temperature standing 24h reacts, reaction finishes rear centrifugal, gets solid phase through washing, oven dry, is titanium dioxide ball.Liquid phase is carried out Distillation recovery, obtains ethanol recycling.
Figure 234635DEST_PATH_IMAGE002
prepare spherical metatitanic acid lithium ion battery negative material: getting concentration is that then 0.25mol/L solubility lithium salt solution 25ml adds 0.6g titanium dioxide ball, ultrasonic dispersion is after 25 minutes, be placed in 180 ℃ of Water Under thermal response 4h, after reaction finishes, product is centrifugal, get solid phase, adopt deionized water and absolute ethyl alcohol to wash respectively three times, after then drying, be placed in again at 800 ℃ and calcine 5h.End product is spherical metatitanic acid lithium ion battery negative material.
embodiment 5
Figure 509759DEST_PATH_IMAGE001
prepare titanium dioxide ball: the solution of the 0.1mol/L potassium chloride of 0.5ml will be added in the absolute ethyl alcohol of 100ml, after stirring with mechanical agitator, drip butyl titanate 2ml, after mechanical agitation 1h, at room temperature standing 24h reacts, reaction finishes rear centrifugal, gets solid phase through washing, oven dry, is titanium dioxide ball.Liquid phase is carried out Distillation recovery, obtains ethanol recycling.
Figure 340181DEST_PATH_IMAGE002
prepare spherical metatitanic acid lithium ion battery negative material: getting concentration is that then 0.7 mol/L solubility lithium salt solution 40ml adds 0.15g titanium dioxide ball, ultrasonic dispersion is after 25 minutes, be placed in 170 ℃ of Water Under thermal response 20h, after reaction finishes, product is centrifugal, get solid phase, adopt deionized water and ethanol to wash respectively three times, after then drying, be placed in again at 700 ℃ and calcine 3h.End product is spherical metatitanic acid lithium ion battery negative material.
Two, product performance:
Fig. 1 is the SEM figure of the titanium dioxide ball that under normal temperature, sol-gel reaction was taken after 24 hours, as seen from Figure 1: titanium dioxide ball smooth in appearance, be of a size of 200-500nm, be uniformly dispersed.
The SEM figure that Fig. 2 is the product of shooting react 15 hours under 180 ℃ of hydrothermal conditions after, as seen from Figure 2, lithium titanate pattern is coccoid, its structure homogeneous is uniformly dispersed, and is of a size of 300-500nm.
Fig. 3 is the XRD figure after 800 ℃ of calcinings react 15 hours under 180 ℃ of hydrothermal conditions after, and by contrast XRD standard card PDF#49-0207, the XRD collection of illustrative plates of this product is consistent with standard spectrum, is spinel type lithium titanate.18.4 ° of diffraction maximums of locating, belong to 111 of lithium titanate, belong to 311 of lithium titanate the diffraction maximums of 35.5 °, the diffraction maximum of 43.2 ° belongs to 400 of lithium titanate, and the diffraction maximum of 62.8 ° belongs to 440 of lithium titanate.
Fig. 4 is the cyclic voltammetry curve figure that product is assembled into rear button cell test, as can be seen from Figure 4, and at 0.2 mVs -1the cyclic voltammetry curve first of spherical lithium titanate under sweep speed, potential range is 1.0-3.0 V.Oxidation peak in figure and reduction peak have good symmetry, show that lithium ion has high transmission rate in spherical lithium titanate.Its charged electric potential platform is 1.6V, and discharge potential platform is 1.5V.
Fig. 5 is the charge-discharge performance figure that product is assembled into rear button cell test, as can be seen from Figure 5, when multiplying power is 1C, discharges and recharges 100 times, and capacity still can reach 120mAh.g -1left and right, cycle performance is more stable.

Claims (8)

1. a preparation method for spherical metatitanic acid lithium ion battery negative material, is characterized in that comprising the following steps:
1) after absolute ethyl alcohol is mixed with potassium chloride solution, then drip butyl titanate, then after mixing, standing reaction at normal temperatures, question response finishes rear centrifugal, gets solid phase washing, dries, and obtains titanium dioxide ball;
2) carry out hydro-thermal reaction after the aqueous solution of solubility lithium salts and titanium dioxide ball are uniformly dispersed in ultrasonic, question response finishes rear centrifugal, gets solid phase washing, dries, and then calcining, obtains spherical metatitanic acid lithium ion battery negative material.
2. preparation method according to claim 1, the concentration that it is characterized in that described potassium chloride solution is 0.1mol/L.
3. preparation method according to claim 1, the volume ratio that feeds intake that it is characterized in that described absolute ethyl alcohol, potassium chloride solution and butyl titanate is 100～200 ︰ 0.2～1 ︰ 2～3.
4. preparation method according to claim 1, is characterized in that described solubility lithium salts is LiOH.H 2o, Li 2cO 3or LiCl.
5. according to preparation method described in claim 1 or 4, the concentration that it is characterized in that the aqueous solution of solubility lithium salts is 0.2 mol/L～1mol/L.
6. preparation method according to claim 1, the mass ratio that it is characterized in that solubility lithium salts and titanium dioxide ball is 25～1 ︰ 1.
7. preparation method according to claim 1, is characterized in that the condition of described ultrasonic processing is: 50～55KHz.
8. preparation method according to claim 1, the temperature conditions that it is characterized in that described hydro-thermal reaction is 100 ℃～200 ℃, the time is 2h～24h.
CN201310615695.XA 2013-11-28 2013-11-28 Preparation method of spherical lithium titanate ion battery cathode material Pending CN103594694A (en)

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Cited By (8)

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CN104009236A (en) * 2014-06-10 2014-08-27 华东理工大学 Lithium titanate mesoporous single-crystal nanoparticle/reduced graphene oxide composite material as well as preparation method and application thereof
CN107098384A (en) * 2017-04-06 2017-08-29 武汉理工大学 One kind is based on TiO2The light-operated micron motor of twin crystal phase micro particles and its preparation and control
CN107176622A (en) * 2017-04-28 2017-09-19 中国电力科学研究院 A kind of lithium titanate material and preparation method thereof
CN107507965A (en) * 2016-06-14 2017-12-22 上海杉杉科技有限公司 A kind of preparation method of nano polyaniline-carbonic acid lithium titanate cathode material
CN107628639A (en) * 2017-09-10 2018-01-26 绵阳梨坪科技有限公司 The preparation method of inner porosity spherical lithium titanate ion battery cathode material
CN108448073A (en) * 2018-02-01 2018-08-24 山东理工大学 Lithium ion battery C@TiO2Composite negative pole material and preparation method thereof
CN109244415A (en) * 2018-09-29 2019-01-18 北京泰丰先行新能源科技有限公司 A kind of preparation method of spherical shape carbon coating titanate composite negative pole material
CN110350170A (en) * 2019-06-28 2019-10-18 陕西科技大学 A kind of preparation method of lithium titanate/graphene composite material

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104009236A (en) * 2014-06-10 2014-08-27 华东理工大学 Lithium titanate mesoporous single-crystal nanoparticle/reduced graphene oxide composite material as well as preparation method and application thereof
CN104009236B (en) * 2014-06-10 2016-06-08 华东理工大学 A kind of metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material and its preparation method and application
CN107507965A (en) * 2016-06-14 2017-12-22 上海杉杉科技有限公司 A kind of preparation method of nano polyaniline-carbonic acid lithium titanate cathode material
CN107098384A (en) * 2017-04-06 2017-08-29 武汉理工大学 One kind is based on TiO2The light-operated micron motor of twin crystal phase micro particles and its preparation and control
CN107176622A (en) * 2017-04-28 2017-09-19 中国电力科学研究院 A kind of lithium titanate material and preparation method thereof
CN107628639A (en) * 2017-09-10 2018-01-26 绵阳梨坪科技有限公司 The preparation method of inner porosity spherical lithium titanate ion battery cathode material
CN108448073A (en) * 2018-02-01 2018-08-24 山东理工大学 Lithium ion battery C@TiO2Composite negative pole material and preparation method thereof
CN109244415A (en) * 2018-09-29 2019-01-18 北京泰丰先行新能源科技有限公司 A kind of preparation method of spherical shape carbon coating titanate composite negative pole material
CN110350170A (en) * 2019-06-28 2019-10-18 陕西科技大学 A kind of preparation method of lithium titanate/graphene composite material

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Application publication date: 20140219