CN107946554A - A kind of preparation method of lithium battery lithium titanate anode material - Google Patents
A kind of preparation method of lithium battery lithium titanate anode material Download PDFInfo
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- CN107946554A CN107946554A CN201711016721.1A CN201711016721A CN107946554A CN 107946554 A CN107946554 A CN 107946554A CN 201711016721 A CN201711016721 A CN 201711016721A CN 107946554 A CN107946554 A CN 107946554A
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- H01M4/02—Electrodes composed of, or comprising, active material
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- 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
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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
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- 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
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Abstract
The present invention provides a kind of preparation method of lithium battery lithium titanate anode material, including：It is the first step, carbon source, lithium source, complexing agent and organic titanium source is soluble in water, and 12 24h of hydro-thermal reaction at 120 200 DEG C；Second step, the product for obtaining the first step are dried；3rd step, by the product that second step obtains roast 2 12h at 700 900 DEG C.The preparation method can Effective Regulation produce lithium titanate material granular size, produce the more homogeneous particle of particle diameter smaller, obtained electrode material granular size is controllable, and carbon coating is uniformly and excellent with high electron conduction, high circulation stability, high power capacity, high power charging-discharging and security performance.
Description
Technical field
The invention belongs to electrode material of lithium battery technical field, more particularly, to a kind of lithium battery lithium titanate anode material
Preparation method.
Background technology
As a kind of lithium cell cathode material, the unit cell volume in charge and discharge process hardly changes lithium titanate, has
The title of " zero strain " material, its capacity attenuation is slow, has good circulation, high power charging-discharging and security performance, has very
Wide application prospect.
But there are particle is thick, electrical conductivity is low and Ti-O keys cause carbon in electrolyte for lithium titanate prepared by currently available technology
Acid esters solute decompose flatulence the problems such as, so as to get lithium titanate anode material electron conduction it is low, cyclical stability is poor, capacity
Low, high power charging-discharging and poor safety performance, have seriously affected the industrial applications of lithium titanate.Have researcher attempt by using
The methods of solid ball milling, to improve lithium carbonate specific capacity and the problem of suppress its aerogenesis, but there are technique to answer to lithium titanate bag carbon
Miscellaneous, the problems such as cladding is uneven.
The content of the invention
The problem to be solved in the present invention is to provide a kind of preparation method of lithium battery lithium titanate anode material, obtained titanium
Sour lithium titanate cathode material particle is homogeneous, size is small, and electron conduction is high, cyclical stability is strong, capacity is high, high power charging-discharging and peace
Full excellent performance.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of lithium battery lithium titanate anode material
Preparation method, including：Step 1: carbon source, lithium source, complexing agent and organic titanium source is soluble in water, and the water at 120-200 DEG C
Thermal response 12-24h；Second step, the product for obtaining the first step are dried；3rd step, the product for obtaining second step are in 700-900
2-12h is roasted at DEG C.
In technical solution, it is preferred that each material molar ratio is carbon source：Lithium source：Complexing agent：Organic titanium source：Water is 0.01-
10：3.5-4.5：5-20：5：100-200.
In technical solution, it is preferred that complexing agent is isopropanol, acetylacetone,2,4-pentanedione, diethanol amine, hydrogen peroxide, urea peroxide
With the one or more in Peracetic acid.
In technical solution, it is preferred that organic titanium source is tetraethyl titanate, butyl titanate, titanium tetraisopropylate and metatitanic acid first
One or more in ester.
In technical solution, it is preferred that carbon source is citric acid, sucrose, glucose, fructose, maltose, lactose, graphene, oxygen
One or more in graphite alkene and carbon nanotubes.
In technical solution, it is preferred that lithium source is lithium carbonate, lithium hydroxide, lithium chloride, lithium oxalate, lithium acetate and citric acid
One or more in lithium.
In technical solution, it is preferred that in the first step, first by carbon source, lithium source and complexing agent formation solution soluble in water, then
Organic titanium source is added dropwise into solution.
In technical solution, it is preferred that in the first step, solution is stirred during organic titanium source is added dropwise.
In technical solution, it is preferred that in the 3rd step, inert gas is passed through during roasting；Preferably, inert gas is
One or more in nitrogen, argon gas, helium.
In technical solution, it is preferred that in second step, the product of the first step is dried using spray drying process.
The present invention has the advantages and positive effects of：This method prepares carbon-coated lithium titanate material using hydrothermal synthesis method
Material, using organic titanium source as titanium source during Hydrothermal Synthesiss, by the hydrolysis of organic titanium source in a solvent, produces titanium dioxide precipitation, can
The particle of smaller is produced, makes contact of the titanium dioxide granule with lithium source evenly, reaction is more abundant；And the complexing agent and water added
Complexing occurs between the titanium solved, the hydrolysis rate of controllable organic titanium source, prevents that organic titanium source is hydrolyzed in a solvent
It hurry up, cause titanium dioxide precipitation to accumulate, cannot come into full contact with reaction with lithium source and material particle size is uncontrollable, further optimization produces
Lithium titanate material particle size, produce the more homogeneous particle of particle diameter smaller, so as to get the big I of electrode material granules
Control, carbon coating are uniformly and excellent with high electron conduction, high circulation stability, high power capacity, high power charging-discharging and security performance
It is different.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph for the lithium titanate material that art methods are prepared.
Fig. 2 is the scanning electron microscope (SEM) photograph for the lithium titanate material being prepared in embodiment one.
Fig. 3 is the scanning electron microscope (SEM) photograph for the lithium titanate material being prepared in embodiment two.
Fig. 4 is the scanning electron microscope (SEM) photograph for the lithium titanate material being prepared in embodiment three.
Fig. 5 is the scanning electron microscope (SEM) photograph for the lithium titanate material being prepared in example IV.
Fig. 6 is the scanning electron microscope (SEM) photograph for the lithium titanate material being prepared in embodiment five.
Embodiment
Lithium titanate is prepared to the methods of lithium titanate bag carbon usually through solid ball-milling method or sol-gal process in the prior art to bear
Pole material, but the obtained lithium titanate material of the prior art is thick there are particle and heterogeneity (prior art as shown in Figure 1 obtains
Lithium titanate material SEM figures), electrical conductivity is low and Ti-O keys cause the problems such as carbonic ester solute decomposes flatulence in electrolyte, its electricity
Subconductivity is low, cyclical stability is poor, capacity is low, high power charging-discharging and poor safety performance.
To solve the above problems, the present invention provides a kind of preparation method of lithium battery lithium titanate anode material, including：
Step 1: carbon source, lithium source, complexing agent and organic titanium source are dissolved in solvent, and the hydro-thermal reaction 12-24h at 120-200 DEG C；
Second step, the product for obtaining the first step are dried；3rd step, by the product that second step obtains roast 2- at 700-900 DEG C
12h.This method prepares carbon-coated lithium titanate material using hydrothermal synthesis method, using organic titanium source as titanium source during Hydrothermal Synthesiss, has
Machine titanium source gradually hydrolyzes in a solvent, and gradually produces titanium dioxide precipitation, compared to directly use titanium dioxide granule for,
The particle of smaller can be produced by producing titanium dioxide by the hydrolysis of organic titanium source, and contact of the titanium dioxide granule with lithium source is more
Uniformly, react more abundant；And complexing can occur between the complexing agent and the titanium of hydrolysis added, controllable organic titanium source
Hydrolysis rate, it is too fast to prevent that organic titanium source from hydrolyzing in a solvent, causes titanium dioxide precipitation to accumulate, cannot be come into full contact with lithium source
Reaction and material particle size are uncontrollable, further the size of the particle for the lithium titanate material that optimization produces, and it is more equal to produce particle diameter smaller
One particle, so as to get electrode material granules size it is controllable, carbon coating uniformly and with high electron conduction, high circulation stablize
Property, high power capacity, high power charging-discharging and security performance are excellent.
Wherein each material molar ratio is carbon source：Lithium source：Complexing agent：Organic titanium source：Water is 0.01-10：3.5-4.5：5-20：
5：100-200.
Complexing agent is mainly that complexing occurs for the titanium produced with organic titanium source ionization, so as to regulate and control the hydrolysis of organic titanium source
Speed, regulates and controls the size of the titanium dioxide granule of generation, and complexing agent can be isopropanol, acetylacetone,2,4-pentanedione, diethanol amine, peroxidating
One or more in hydrogen, urea peroxide and Peracetic acid.
Organic titanium source can slowly hydrolyze in aqueous solvent, produce titanium dioxide precipitation, and organic titanium source can select
One or more in tetraethyl titanate, butyl titanate, titanium tetraisopropylate and metatitanic acid methyl esters.
Carbon source can select citric acid, sucrose, glucose, fructose, maltose, lactose, graphene, graphene oxide and carbon
One or more in nanotube.
Lithium source can select one kind in lithium carbonate, lithium hydroxide, lithium chloride, lithium oxalate, lithium acetate and lithium citrate or
It is several.
In this method, preferable method, in the first step, first carbon source, lithium source and complexing agent are dissolved in solvent formed it is molten
Liquid, is then added dropwise organic titanium source into solution, can so make the concentration of titanium source in solution relatively low, increases titanium source and the complexing of addition
The uniformity of the contact of agent, makes the speed for producing titanium dioxide precipitation in solution slower, produces the more homogeneous metatitanic acid of granularity smaller
Lithium material particle, and make titanium source, the mixing of lithium source and reaction evenly.
It is furthermore preferred that in the first step, solution is constantly stirred during organic titanium source is added dropwise, make titanium source and
The mixing of complexing agent is evenly.
In preferred solution, in the 3rd step, inert gas is passed through during roasting；Inert gas is to the ring to roasting process
Border shields, and prevents having oxygen etc. can be at high temperature with treating to react between calcined material in environment.Preferably, inertia
Gas is nitrogen, the one or more in argon gas, helium.
In preferred solution, in second step, the product of the first step is dried and is done using spray drying process, spray drying process
Dry efficient, drying effect is more homogeneous.
Describe in detail with reference to specific embodiment to embodiments of the present invention：
Embodiment one
2g sucrose and 9.58g lithium hydroxides are dissolved into 180g water, add the H of 38.7g 30wt%2O2, stirring
15min, obtains material 1；Take 97.2g butyl titanates to be slowly dropped under stirring in material 1, obtain material 2；By material
2 are put into 500ml hydrothermal reaction kettles, and constant temperature keeps 12h at 180 DEG C, obtains material 3, are spray-dried, obtain material 4；By material
4 under nitrogen protection 750 DEG C roasting 8h, you can obtain lithium battery lithium titanate material, obtained lithium titanate material use swept
Retouch Electronic Speculum to be observed, such as the stereoscan photograph that Fig. 2 is the lithium titanate material that the present embodiment obtains.
Lithium ion battery is prepared as active material using lithium titanate material made from the present embodiment.Using 1-methyl-2-pyrrolidinone as
Solvent, lithium titanate material and conductive additive Super-P Li and binding agent Kynoar in mass ratio 8:1:1 is stirred
Slurry is prepared after uniformly, is then coated with Al paper tinsels, is cold-pressed after drying and is washed into 10mm diameter discs.Disk and lithium metal is made
Button electricity is made in piece, and membrane is that Celgard2400 is sky polypropylene screen, and electrolyte is the LiPF6 solution of 1M.After detaining stating in atelegran 12h
Constant current charge-discharge test is carried out, first discharge specific capacity reaches 163mAh/g, and capacity is protected after being circulated 100 times under 200mA/h multiplying powers
Holdup is 95%.
Observed result from scanning electron microscope and the electrical test results using lithium ion battery made from this material, by
The granular size smaller for the lithium titanate material that the method obtains and more homogeneous, electron conduction is high, cyclical stability is strong, high magnification
Discharge and recharge and security performance are excellent.
Embodiment two
5g fructose and 9.58g lithium hydroxides are dissolved into 180g water, add 192.4g isopropanols, 15min is stirred, obtains
To material 1；Take 65.6g tetraethyl titanates to be slowly dropped under stirring in material 1, obtain material 2；Material 2 is put into
In 500ml hydrothermal reaction kettles, constant temperature keeps 24h at 150 DEG C, obtains material 3, is spray-dried, obtains material 4；By material 4 in argon
The lower 800 DEG C of roastings 6h of gas shielded, you can obtain lithium battery lithium titanate material, scanning electron microscope is used to obtained lithium titanate material
It is observed, such as the stereoscan photograph that Fig. 3 is the lithium titanate material that the present embodiment obtains.
Lithium ion battery is prepared as active material using lithium titanate material made from the present embodiment.Using 1-methyl-2-pyrrolidinone as
Solvent, lithium titanate material and conductive additive Super-P Li and binding agent Kynoar in mass ratio 8:1:1 is stirred
Slurry is prepared after uniformly, is then coated with, in Al paper tinsels, being cold-pressed after drying and being washed into 10mm diameter discs.Disk and metal lithium sheet is made
Button electricity is made, membrane is that Celgard 2400 is sky polypropylene screen, and electrolyte is the LiPF6 solution of 1M.It is laggard to detain stating in atelegran 12h
Row constant current charge-discharge test, first discharge specific capacity reach 156mAh/g, and capacity is kept after being circulated 100 times under 200mA/h multiplying powers
Rate is 93%.
Observed result from scanning electron microscope and the electrical test results using lithium ion battery made from this material, by
The granular size smaller for the lithium titanate material that the method obtains and more homogeneous, electron conduction is high, cyclical stability is strong, high magnification
Discharge and recharge and security performance are excellent.
Embodiment three
10g glucose and 27.5g lithium carbonates are dissolved into 180g water, add 100g acetylacetone,2,4-pentanediones, stirs 15min,
Obtain material 1；Take 81.7g titanium tetraisopropylates to be slowly dropped under stirring in material 1, obtain material 2；Material 2 is put into
In 500ml hydrothermal reaction kettles, constant temperature keeps 12h at 200 DEG C, obtains material 3, is spray-dried, obtains material 4；By material 4 in helium
The lower 900 DEG C of roastings 4h of gas shielded, you can obtain lithium battery lithium titanate material, scanning electron microscope is used to obtained lithium titanate material
It is observed, such as the stereoscan photograph that Fig. 4 is the lithium titanate material that the present embodiment obtains.
Lithium ion battery is prepared as active material using lithium titanate material made from the present embodiment.Using 1-methyl-2-pyrrolidinone as
Solvent, lithium titanate material and conductive additive Super-P Li and binding agent Kynoar in mass ratio 8:1:1 is stirred
Slurry is prepared after uniformly, is then coated with, in Al paper tinsels, being cold-pressed after drying and being washed into 10mm diameter discs.Disk and metal lithium sheet is made
Button electricity is made, membrane is that Celgard 2400 is sky polypropylene screen, and electrolyte is the LiPF6 solution of 1M.It is laggard to detain stating in atelegran 12h
Row constant current charge-discharge test, first discharge specific capacity reach 168mAh/g, and capacity is kept after being circulated 100 times under 200mA/h multiplying powers
Rate is 92%.
Observed result from scanning electron microscope and the electrical test results using lithium ion battery made from this material, by
The granular size smaller for the lithium titanate material that the method obtains and more homogeneous, electron conduction is high, cyclical stability is strong, high magnification
Discharge and recharge and security performance are excellent.
Example IV
2g maltose and 37.5g lithium citrates are dissolved into 180g water, 94.1g 50wt% urea peroxides is added, stirs
15min is mixed, obtains material 1；Take 97.2g butyl titanates to be slowly dropped under stirring in material 1, obtain material 2；By thing
Material 2 is put into 500ml hydrothermal reaction kettles, and constant temperature keeps 24h at 150 DEG C, obtains material 3, is spray-dried, is obtained material 4；By thing
The 800 DEG C of roasting 6h under argon gas protection of material 4, you can obtain lithium battery lithium titanate material, use obtained lithium titanate material
Scanning electron microscope is observed, such as the stereoscan photograph that Fig. 5 is the lithium titanate material that the present embodiment obtains.
Lithium ion battery is prepared as active material using lithium titanate material made from the present embodiment.Using 1-methyl-2-pyrrolidinone as
Solvent, lithium titanate material and conductive additive Super-P Li and binding agent Kynoar in mass ratio 8:1:1 is stirred
Slurry is prepared after uniformly, is then coated with, in Al paper tinsels, being cold-pressed after drying and being washed into 10mm diameter discs.Disk and metal lithium sheet is made
Button electricity is made, membrane is that Celgard 2400 is sky polypropylene screen, and electrolyte is the LiPF6 solution of 1M.It is laggard to detain stating in atelegran 12h
Row constant current charge-discharge test, first discharge specific capacity reach 160mAh/g, and capacity is kept after being circulated 100 times under 200mA/h multiplying powers
Rate is 90%.
Observed result from scanning electron microscope and the electrical test results using lithium ion battery made from this material, by
The granular size smaller for the lithium titanate material that the method obtains and more homogeneous, electron conduction is high, cyclical stability is strong, high magnification
Discharge and recharge and security performance are excellent.
Embodiment five
15g lactose and 9.58g lithium hydroxides are dissolved into 180g water, add 52.5g diethanol amine, stirs 15min,
Obtain material 1；Take 65.6g tetraethyl titanates to be slowly dropped under stirring in material 1, obtain material 2；Material 2 is put into
In 500ml hydrothermal reaction kettles, constant temperature keeps 12h at 180 DEG C, obtains material 3, is spray-dried, obtains material 4；By material 4 in nitrogen
The lower 700 DEG C of roastings 8h of gas shielded, you can obtain lithium battery lithium titanate material, scanning electron microscope is used to obtained lithium titanate material
It is observed, such as the stereoscan photograph that Fig. 6 is the lithium titanate material that the present embodiment obtains.
Lithium ion battery is prepared as active material using lithium titanate material made from the present embodiment.Using 1-methyl-2-pyrrolidinone as
Solvent, lithium titanate material and conductive additive Super-P Li and binding agent Kynoar in mass ratio 8:1:1 is stirred
Slurry is prepared after uniformly, is then coated with, in Al paper tinsels, being cold-pressed after drying and being washed into 10mm diameter discs.Disk and metal lithium sheet is made
Button electricity is made, membrane is that Celgard 2400 is sky polypropylene screen, and electrolyte is the LiPF6 solution of 1M.It is laggard to detain stating in atelegran 12h
Row constant current charge-discharge test, first discharge specific capacity reach 172mAh/g, and capacity is kept after being circulated 100 times under 200mA/h multiplying powers
Rate is 100%.
Observed result from scanning electron microscope and the electrical test results using lithium ion battery made from this material, by
The granular size smaller for the lithium titanate material that the method obtains and more homogeneous, electron conduction is high, cyclical stability is strong, high magnification
Discharge and recharge and security performance are excellent.
Several embodiments of the present invention are described in detail above, but the content is only the preferable implementation of the present invention
Example, it is impossible to be construed as limiting the practical range of the present invention.All all the changes and improvements made according to the present patent application scope
Deng, should all still belong to the present invention patent covering scope within.
Claims (10)
- A kind of 1. preparation method of lithium battery lithium titanate anode material, it is characterised in that：Including：The first step, by carbon source, lithium Source, complexing agent and organic titanium source are soluble in water, and the hydro-thermal reaction 12-24h at 120-200 DEG C；Second step, obtain the first step Product drying；3rd step, by the product that second step obtains roast 2-12h at 700-900 DEG C.
- 2. the preparation method of negative material according to claim 1, it is characterised in that：Each material molar ratio is carbon source：Lithium Source：Complexing agent：Organic titanium source：Water is 0.01-10：3.5-4.5：5-20：5：100-200.
- 3. the preparation method of negative material according to claim 1 or 2, it is characterised in that：The complexing agent for isopropanol, One or more in acetylacetone,2,4-pentanedione, diethanol amine, hydrogen peroxide, urea peroxide and Peracetic acid.
- 4. according to the preparation method of any negative materials of claim 1-3, it is characterised in that：The organic titanium source is titanium One or more in sour tetra-ethyl ester, butyl titanate, titanium tetraisopropylate and metatitanic acid methyl esters.
- 5. according to the preparation method of any negative materials of claim 1-4, it is characterised in that：The carbon source is lemon One or more in acid, sucrose, glucose, fructose, maltose, lactose, graphene, graphene oxide and carbon nanotubes.
- 6. according to the preparation method of any negative materials of claim 1-5, it is characterised in that：The lithium source is carbonic acid One or more in lithium, lithium hydroxide, lithium chloride, lithium oxalate, lithium acetate and lithium citrate.
- 7. according to the preparation method of any negative materials of claim 1-6, it is characterised in that：In the first step, first By the carbon source, the lithium source and complexing agent formation solution soluble in water, then it is added dropwise into the solution described organic Titanium source.
- 8. the preparation method of negative material according to claim 7, it is characterised in that：In the first step, described in dropwise addition The solution is stirred during organic titanium source.
- 9. according to the preparation method of any negative materials of claim 1-8, it is characterised in that：In 3rd step, roasting Inert gas is passed through during burning；Preferably, the inert gas is the one or more in nitrogen, argon gas, helium.
- 10. according to the preparation method of any negative materials of claim 1-9, it is characterised in that：It is right in the second step The product of the first step is dried using spray drying process.
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| CN109768264A (en) * | 2019-03-06 | 2019-05-17 | 浙江工业大学 | A kind of preparation method of lithium titanate composite anode material |
| CN109802106A (en) * | 2018-12-25 | 2019-05-24 | 江苏理工学院 | A kind of method of electrode material surface modification |
| CN110611078A (en) * | 2018-06-14 | 2019-12-24 | 浙江伏打科技有限公司 | Preparation method of lithium titanate-carbon nanotube electrode material |
| CN114180567A (en) * | 2021-12-20 | 2022-03-15 | 江苏恒贵信新材料有限公司 | Vertical graphitizing furnace with rapid cooling function |
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