CN102009998A - Method for preparing lithium ion battery cathode material lithium titanate - Google Patents

Method for preparing lithium ion battery cathode material lithium titanate Download PDF

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Publication number
CN102009998A
CN102009998A CN2010105227085A CN201010522708A CN102009998A CN 102009998 A CN102009998 A CN 102009998A CN 2010105227085 A CN2010105227085 A CN 2010105227085A CN 201010522708 A CN201010522708 A CN 201010522708A CN 102009998 A CN102009998 A CN 102009998A
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lithium
tio
preparation
cathode material
constant temperature
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韩恩山
朱令之
张俊平
靳素芳
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Hebei University of Technology
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    • 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 method for preparing a lithium ion battery cathode material lithium titanate. The method comprises the following steps of: mixing lithium source, TiO2 and carbonization agent uniformly, wherein the molar ratio of Li to Ti is 0.80-0.88:1 and the mass ratio of the TiO2 to the carbonization agent is 4-8: 1; adding the mixture into 0.15 to 0.2 percent aqueous solution of polyacrylamide (PAM), wherein the mass ratio of the PAM to the TiO2 is 0.002-0.003:1; and intensely stirring and uniformly mixing the materials, keeping the materials at a constant temperature of 100 DEG C for 3 hours in a muffle furnace, pre-calcining the materials at 600 DEG C, keeping the pre-calcined product at a constant temperature for 12 hours, cooling the pre-calcined product together with the furnace, grinding the pre-calcined product into powder, and calcining the powder for 16 hours at the temperature of between 750 and 950 DEG C in the muffle furnace to obtain a product. The first discharge capacity of the Li4Ti5O12 material reaches 170mAh/g, the capacity nearly has no attenuation after 20 times of cycles, the polarization of the material is reduced, and the electrochemical performance of the material is excellent.

Description

A kind of preparation method of lithium ionic cell cathode material lithium titanate
Technical field
The present invention relates to the battery material preparing technical field, be specially a kind of preparation method of lithium ionic cell cathode material lithium titanate.
Background technology
Lithium ion battery is a kind of novel rechargeable cell, its energy density per unit volume and specific energy height, can fill and pollution-free, the three big advantages that possessed current battery industry development, be referred to as by people by " the most promising chemical power source ", thereby just be subjected to people's extensive concern once coming out, develop very fast.Being widely used in various portable type electronic products and communication tool in recent years, and progressively being developed as the electrical source of power of electromobile, is the new forms of energy of safety and environmental protection.
The successful commercialization of lithium ion battery is mainly given the credit to lithium intercalation compound and is replaced lithium anode.Researching and developing new electrochemistry can better negative material be the heat subject in Study on Li-ion batteries using field.Lithium ion battery negative material adopts embedding lithium carbon material mostly at present.The advantage of graphite material is wide material sources, low price, and the charging/discharging voltage platform is low, reversible capacity height (theoretical value 372mAhg).But graphite and solvent compatibility are poor, and high rate during charging-discharging is bad, and the common embedding because of solvent molecule during first charge-discharge is peeled off graphite linings, thereby cause electrode cycle life to reduce.In order to solve the various defectives that current material exists, battery circle has been done big quantity research, carbon negative pole material is being carried out various improvement with when improving its performance, and the development of new negative material also is the focus of paying close attention to always.Therefore seek the desirable negative active core-shell material of lithium ion battery from resource, environmental protection and safety performance aspect, be still the research focus of for some time World chemical power supply circle from now on.
1996, Canadian Studies person K.zaghib proposes to adopt lithium titanate material to make negative pole first and high-voltage anode is formed lithium-ions battery, formed electrochemical mixed capacitor with carbon electrode.Afterwards, little bavin letter was fine waits the people also it to be carried out research as ion cathode material lithium.Calendar year 2001, Li such as G.G.Amatucci 4Ti 5O 12The negative pole that replaces double layer capacitor uses electrolyte for lithium cells, has obtained the energy density of 20wh/kg.After this, people are to Li 4Ti 5O 12Begun a large amount of research as negative material.Toshiba Corp announced that exploitation was based on Li in 2007 4Ti 5O 12Lithium ion battery " SCiB ", be intended to be used for the hybrid power field.U.S. Enerdel company has also showed Li in the AABC-07 meeting 4Ti 5O 12The hybrid vehicle lithium ion battery.
Li 4Ti 5O 12Has lot of advantages as lithium ion battery negative material: (1) Li 4Ti 5O 12The theoretical specific capacity height, be 175mAh/g; (2) its skeleton structure is almost constant in charge and discharge process, has " zero strain " characteristic, thereby stable cycle performance; (3) embedding lithium current potential height (1.55vs.Li/Li +) and be difficult for causing that metallic lithium separates out, eliminated potential safety hazard; (4) Li 4Ti 5O 12In, lithium ion spread coefficient (2 * 10 -8Cm 2/ s) be about in the graphite 10 times, have the large current density electrical dominance.Titanium resource is abundant simultaneously, and is cheap, thereby, Li 4Ti 5O 12It is lithium ion battery ideal negative pole candidate material.
At present, the method for preparing lithium titanate material has a lot, and what the research use was maximum is high temperature solid-state method, and it is easy and simple to handle, easily realizes suitability for industrialized production.But solid phase method commonly used divides two kinds, and a kind of is directly raw material to be mixed, and calcines, and the material granule that obtains like this is bigger, and size distribution is inhomogeneous, the chemical property instability; Another kind is in order to obtain the particle of small particle size, and often adopt mechanical ball milling, sieve etc. carried out pre-treatment to raw material, makes the building-up process complexity, thereby production cost is increased.
Summary of the invention:
The present invention is directed to the high temperature solid-state method weak point, by using cheap titanium dioxide to be the titanium source, by with lithium salts, titanium dioxide, the disposable mixing of carbonized agent, avoided complicated feed way, in presoma, add an amount of solvent, the material brute force is stirred, realize the mixing and the mutual parcel of material molecular level, calcining has prepared the good Li of chemical property through two steps 4Ti 5O 12Negative material.Reduce the cost of building-up process, made it to be easy to realize industrialization.
Technical scheme of the present invention is:
A kind of preparation method of lithium ionic cell cathode material lithium titanate may further comprise the steps:
With lithium source, TiO 2Mix with carbonized agent, its material proportion is mol ratio Li: Ti=0.80～0.88: 1, mass ratio TiO 2: carbonized agent=4～8: 1, then mixture is joined concentration and be in 0.15%～0.2% polyacrylamide (PAM) aqueous solution, its quality proportioning is polyacrylamide: TiO 2=0.002～0.003: 1, powerful then the stirring is after mixing, with material 100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, grind into powder, 750～950 ℃ of calcining 16h in retort furnace make product then.
Among the described preparation method, in the raw material except lithium source, TiO 2And carbonized agent, also add Na 2CO 3, mol ratio Na: Ti=0.01～0.10: 5 wherein;
Among the described preparation method, in the raw material except lithium source, TiO 2And carbonized agent, also add manganous acetate, wherein mol ratio Mn: Li=0.01～0.12: 4;
Described lithium source is Quilonum Retard or lithium hydroxide;
Described carbonized agent is gac, citric acid or glucose.
Beneficial effect of the present invention is: the present invention makes carbonized agent by adding a certain amount of carbon source, has stoped Li on microcosmic 4Ti 5O 12Nucleus growth excessive, and in calcination process, generate CO 2Gas is discharged, and has suppressed the particulate reunion.Adopt the PAM aqueous solution to make solvent, raw material is mixed under solution environmental, contact is more abundant, more even between the feed particles.The Li that obtains 4Ti 5O 12Material loading capacity first reaches 170mAh/g, and near theoretical capacity, particle diameter is little, be evenly distributed, and median size is approximately 100～400nm, and particle is more little, helps Li +Embedding and deviate from, make material have good cycle performance, almost do not decay through 20 circulation back capacity, polarization reduces, chemical property is good.
Be elaborated below in conjunction with embodiment and accompanying drawing.
Description of drawings
Accompanying drawing 1 is the X ray diffracting spectrum of the product of embodiment 2, embodiment 5 and embodiment 6 preparations;
Accompanying drawing 2 is the SEM figure of the product for preparing under embodiment 1,2,3,4 differing tempss;
Accompanying drawing 3 is the first charge-discharge specific storage curve of product under 0.1C of embodiment 2, embodiment 5 and embodiment 6 preparations;
Accompanying drawing 4 is mixed Na product Li for the lithium position of embodiment 5 preparations 3.97Na 0.03Ti 5O 12SEM figure;
Accompanying drawing 5 is mixed Mn product Li for the titanium position of embodiment 6 preparations 4Ti 4.96Mn 0.04O 12SEM figure;
Accompanying drawing 6 is the first charge-discharge specific storage curve of product under 0.1C of embodiment 2, embodiment 5 and embodiment 6 preparations;
Accompanying drawing 7 is the cycle performance curve of product under 0.2C of embodiment 2, embodiment 5 and embodiment 6 preparations;
Accompanying drawing 8 is the first charge-discharge specific storage curve of product under 0.1C of embodiment 7 preparations.
Embodiment
Embodiment 1
Take by weighing 1.5517g (0.021mol) Li 2CO 3, 3.9935g (0.05mol) TiO 2, the 1.0g citric acid, the three is vibrated in little Plastic Bottle and is mixed.Take by weighing polyacrylamide 0.01g and place crucible, add the 5ml redistilled water, treat that it fully dissolves, form polyacrylamide solution.Above three's mixture is joined in the polyacrylamide solution, and brute force stirs, and forms the rheology phase of pasty state.100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, and grind into powder is calcined 16h at 800 ℃ then in retort furnace, make pure phase Li 4Ti 5O 12Product.
Embodiment 2
Take by weighing 1.5517g (0.021mol) Li 2CO 3, 3.9935g (0.05mol) TiO 2, the 1.0g citric acid, the three is vibrated in little Plastic Bottle and is mixed.Take by weighing polyacrylamide 0.01g and place crucible, add the 5ml redistilled water, treat that it fully dissolves, form polyacrylamide solution.Above three's mixture is joined in the polyacrylamide solution, and brute force stirs, and forms the rheology phase of pasty state.100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, and grind into powder is calcined 16h at 850 ℃ then in retort furnace, make pure phase Li 4Ti 5O 12Product.
Embodiment 3
Take by weighing 1.5517g (0.021mol) Li 2CO 3, 3.9935g (0.05mol) TiO 2, the 1.0g citric acid, the three is vibrated in little Plastic Bottle and is mixed.Take by weighing polyacrylamide 0.01g and place crucible, add the 5ml redistilled water, treat that it fully dissolves, form polyacrylamide solution.Above three's mixture is joined in the polyacrylamide solution, and brute force stirs, and forms the rheology phase of pasty state.100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, and grind into powder is calcined 16h at 900 ℃ then in retort furnace, make pure phase Li 4Ti 5O 12Product.
Embodiment 4
Take by weighing 1.5517g (0.021mol) Li 2CO 3, 3.9935g (0.05mol) TiO 2, the 1.0g citric acid, the three is vibrated in little Plastic Bottle and is mixed.Take by weighing polyacrylamide 0.01g and place crucible, add the 5ml redistilled water, treat that it fully dissolves, form polyacrylamide solution.Above three's mixture is joined in the polyacrylamide solution, and brute force stirs, and forms the rheology phase of pasty state.100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, and grind into powder is calcined 16h at 950 ℃ then in retort furnace, make pure phase Li 4Ti 5O 12Product.
The product of preparing is made the electrode slice of simulated battery: take by weighing active material Li at 80: 10: 10 by mass ratio 4Ti 5O 12, acetylene black, PVDF.With Li 4Ti 5O 12In agate mortar, grind refinement, mixing with acetylene black; Add a certain amount of binder solution (PVDF is dissolved in an amount of N-Methyl pyrrolidone), stir, make slurry, be coated on the Copper Foil.Drying, roll extrusion are washed into disk and the weighing that diameter is 10mm and make electrode.Make counter electrode with metal lithium sheet, Celgard2400 is a barrier film, and 1mol/L LiPF6/EC+DMC+EMC (volume ratio 1: 1: 1) is an electrolytic solution, is assembled into battery in (relative humidity≤4%) glove box of logical dry air, leaves standstill 24h after the battery assembling finishes.
Test carrying out constant current charge-discharge under the battery room temperature with Wuhan gold promise cell tester, through test comparison, the product of 850 ℃ of preparations is better than other temperature, under 0.1C, discharge and recharge, when the charging/discharging voltage scope is 1.0～2.5V, by accompanying drawing 5 as can be known, first discharge specific capacity reaches 170mAh/g, near theoretical capacity (175mAh/g).By XRD spectra in the accompanying drawing 1 as can be known, each diffraction peak is corresponding one by one, and the inclusion-free peak illustrates the spinel type lithium titanate that has obtained pure phase.Accompanying drawing 2 is the SEM photo of the product that obtains under the differing temps, contrast as can be known, the product cut size that product obtains under 800,850 ℃ is less, and evenly, the particle diameter of product becomes big more than 900 ℃, this is possible be because high temperature is reunited particle.
Embodiment 5
Take by weighing 1.5517g (0.021mol) Li 2CO 3, 3.9935g (0.05mol) TiO 2, the 0.50g gac, the three is vibrated in little Plastic Bottle and is mixed.Take by weighing polyacrylamide 0.01g and place crucible, add the 5ml redistilled water, treat that it fully dissolves, form polyacrylamide solution.Above three's mixture is joined in the polyacrylamide solution, and brute force stirs, and forms the rheology phase of pasty state.100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, and grind into powder is calcined 16h at 850 ℃ then in retort furnace, make pure phase Li 4Ti 5O 12Product.
Embodiment 6
Take by weighing 1.5517g (0.021mol) Li 2CO 3, 3.9935g (0.05mol) TiO 2, 1.0g glucose, the three is vibrated in little Plastic Bottle and is mixed.Take by weighing polyacrylamide 0.01g and place crucible, add the 5ml redistilled water, treat that it fully dissolves, form polyacrylamide solution.Above three's mixture is joined in the polyacrylamide solution, and brute force stirs, and forms the rheology phase of pasty state.100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, and grind into powder is calcined 16h at 850 ℃ then in retort furnace, make pure phase Li 4Ti 5O 12Product.
By accompanying drawing 3 as can be known, different carbonized agents are little to the capacity impact of product, and the first charge-discharge specific storage is all more than 162mAh/g.
Embodiment 7
Take by weighing 1.5400g (0.0208mol) Li 2CO 3, 3.9935g (0.05mol) TiO 2, 0.0159g (0.00015mol) Na 2CO 3, the 1.0g citric acid, four vibrate in little Plastic Bottle mixes.Take by weighing polyacrylamide 0.01g and place crucible, add the 5ml redistilled water, treat that it fully dissolves, form polyacrylamide solution.Above three's mixture is joined in the polyacrylamide solution, and brute force stirs, and forms the rheology phase of pasty state.100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, and grind into powder is calcined 16h at 850 ℃ then in retort furnace, make the lithium position and mix Na product Li 3.97Na 0.03Ti 5O 12(doping is considerably less here, does not change original crystalline structure, thus still lithium titanate, the strictness metal-doped lithium titanate of saying so)
Adopt the full-automatic X-ray diffractometer of German buluke D8 Focus to the material phase analysis that product carries out, the XRD figure that obtains product is composed as shown in Figure 1, and sweep limit is 10～90 °.With standard card (PDF-49-0207) contrast, each diffraction peak is corresponding one by one, the inclusion-free peak, illustrate to obtain spinel type crystal, lithium titanate has been carried out effective doping by accompanying drawing 5 as can be known, under 0.1C, discharge and recharge, first discharge specific capacity reaches 158mAh/g, and with the contrast of pure phase product, capacity slightly reduces, this may be the doping of Na, has occupied the Li position, causes the loss of part capacity, but as can be known by accompanying drawing 6, cycle performance increases, through 30 circulations, capacity attenuation minimum.Be the SEM photo of product in the accompanying drawing 3, grain diameter is less, but homogeneity is bad.
Embodiment 8
Take by weighing 1.5400g (0.0208mol) Li 2CO 3, 3.9935g (0.05mol) TiO 2, 0.0987g (0.0004mol) manganous acetate, 1.0g citric acid, four vibrate in little Plastic Bottle mixes.Take by weighing polyacrylamide 0.01g and place crucible, add the 5ml redistilled water, treat that it fully dissolves, form polyacrylamide solution.Above three's mixture is joined in the polyacrylamide solution, and brute force stirs, and forms the rheology phase of pasty state.100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, and grind into powder is calcined 16h at 850 ℃ then in retort furnace, make the titanium position and mix Mn product Li 4Ti 4.96Mn 0.04O 12
Adopt the full-automatic X-ray diffractometer of German buluke D8 Focus to the material phase analysis that product carries out, the XRD figure that obtains product is composed as shown in Figure 1, and sweep limit is 10～90 °.With standard card (PDF-49-0207) contrast, each diffraction peak is corresponding one by one, and the inclusion-free peak illustrates to obtain spinel type crystal, and lithium titanate has been carried out effective doping.By accompanying drawing 5 as can be known, carry out charge-discharge test under 0.1C, first discharge specific capacity reaches 170mAh/g, and by accompanying drawing 6 as can be known, it is better than pure phase product that the cyclic voltammetric test draws cycle performance.
Embodiment 9
Take by weighing 0.96g (0.04mol) LiOH, 3.9935g (0.05mol) TiO 2, the 1.0g citric acid, four vibrate in little Plastic Bottle mixes.Take by weighing polyacrylamide 0.01g and place crucible, add the 5ml redistilled water, treat that it fully dissolves, form polyacrylamide solution.Above three's mixture is joined in the polyacrylamide solution, and brute force stirs, and forms the rheology phase of pasty state.100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, and grind into powder is calcined 16h at 850 ℃ then in retort furnace, make pure phase Li 4Ti 5O 12Product.
The group of products of preparation is dressed up battery, carries out charge-discharge test under 0.1C, as shown in Figure 7, first discharge specific capacity reaches more than the 160mAh/g, capacity is lower than the product (for 170mAh/g) that adopts Quilonum Retard to prepare for the lithium source slightly, and difference is little, and the different lithium source can both draw the product of excellent property.

Claims (5)

1. the preparation method of a lithium ionic cell cathode material lithium titanate is characterized by and may further comprise the steps:
With lithium source, TiO 2Mix with carbonized agent, its material proportion is mol ratio Li: Ti=0.80～0.88: 1, mass ratio TiO 2: carbonized agent=4～8: 1, then mixture is joined concentration and be in 0.15%～0.2% polyacrylamide (PAM) aqueous solution, its quality proportioning is polyacrylamide: TiO 2=0.002～0.003: 1, powerful then the stirring is after mixing, with material 100 ℃ of constant temperature 3h of elder generation in retort furnace, 600 ℃ of pre-burnings, constant temperature 12h cools to room temperature with the furnace again, grind into powder, 750～950 ℃ of calcining 16h in retort furnace make product then.
2. the preparation method of lithium ionic cell cathode material lithium titanate as claimed in claim 1 is characterized by among the described preparation method, in the raw material except lithium source, TiO 2And carbonized agent, also add Na 2CO 3, mol ratio Na: Ti=0.01～0.10: 5 wherein.
3. the preparation method of lithium ionic cell cathode material lithium titanate as claimed in claim 1 is characterized by among the described preparation method, in the raw material except lithium source, TiO 2And carbonized agent, also add manganous acetate, wherein mol ratio Mn: Li=0.01～0.12: 4.
4. the preparation method of lithium ionic cell cathode material lithium titanate as claimed in claim 1, it is characterized by described lithium source is Quilonum Retard or lithium hydroxide.
5. the preparation method of lithium ionic cell cathode material lithium titanate as claimed in claim 1, it is characterized by described carbonized agent is gac, citric acid or glucose.
CN2010105227085A 2010-10-28 2010-10-28 Method for preparing lithium ion battery cathode material lithium titanate Pending CN102009998A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102633300A (en) * 2011-12-07 2012-08-15 天津市贝特瑞新能源材料有限责任公司 Carbon-coated lithium titanate cathode material as well as preparation method and applications thereof
CN103011265A (en) * 2012-12-26 2013-04-03 彩虹集团公司 Preparation method of lithium titanate
CN104037414A (en) * 2014-06-20 2014-09-10 上海动力储能电池系统工程技术有限公司 Modified lithium-titanate material for lithium ion battery and preparation method of modified lithium-titanate material
WO2015045254A1 (en) * 2013-09-25 2015-04-02 三洋電機株式会社 Lithium-titanium compound oxide
CN108615873A (en) * 2018-05-24 2018-10-02 北方奥钛纳米技术有限公司 It mixes the preparation method of tantalum lithium titanate anode material and mixes tantalum lithium titanate anode material and lithium ion battery

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101764207A (en) * 2009-09-25 2010-06-30 合肥工业大学 Lithium titanate for lithium ion battery negative electrode material and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101764207A (en) * 2009-09-25 2010-06-30 合肥工业大学 Lithium titanate for lithium ion battery negative electrode material and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102633300A (en) * 2011-12-07 2012-08-15 天津市贝特瑞新能源材料有限责任公司 Carbon-coated lithium titanate cathode material as well as preparation method and applications thereof
CN103011265A (en) * 2012-12-26 2013-04-03 彩虹集团公司 Preparation method of lithium titanate
WO2015045254A1 (en) * 2013-09-25 2015-04-02 三洋電機株式会社 Lithium-titanium compound oxide
CN104037414A (en) * 2014-06-20 2014-09-10 上海动力储能电池系统工程技术有限公司 Modified lithium-titanate material for lithium ion battery and preparation method of modified lithium-titanate material
CN108615873A (en) * 2018-05-24 2018-10-02 北方奥钛纳米技术有限公司 It mixes the preparation method of tantalum lithium titanate anode material and mixes tantalum lithium titanate anode material and lithium ion battery

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Application publication date: 20110413