CN104810513B - A kind of lithium ion battery negative material and preparation method thereof - Google Patents
A kind of lithium ion battery negative material and preparation method thereof Download PDFInfo
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- CN104810513B CN104810513B CN201510147348.8A CN201510147348A CN104810513B CN 104810513 B CN104810513 B CN 104810513B CN 201510147348 A CN201510147348 A CN 201510147348A CN 104810513 B CN104810513 B CN 104810513B
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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
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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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Abstract
The invention discloses a kind of lithium ion battery negative material, its chemical formula is Li2TiSiO5, it is α VPO5Structure, with three dimensions layer structure；Under room temperature condition, constant current charge-discharge test is carried out with 10mA/g current density in the range of 0.01~2.0V, the reversible capacity for obtaining its charge and discharge process is more than 180mAh/g, and the platform for taking off lithium process is 0.68~0.75V, and the platform of process of intercalation is 0.28~0.35V.The titanium silicate lithium material of the present invention as lithium ion battery negative pole when, be prevented effectively from caused by polarization negative pole and analyse lithium problem, can greatly improve the security performance of battery；Relative to lithium ion battery of the lithium titanate as negative pole is used, using its charging/discharging voltage wider range during titanium silicate lithium, capacity is high, and the energy density of battery is highly improved, and cycle performance of battery is excellent；Material produced by the present invention has more gentle charge and discharge platform.
Description
Technical field
New titanium silicate lithium is used for lithium ion battery the present invention relates to field of lithium ion battery material, more particularly to one kind
The preparation method of negative material.
Background technology
Lithium ion battery belongs to secondary cell, because it has a high power density, high-energy-density, cycle performance it is excellent with
And the advantage such as temperature in use scope is wide, have been widely used for electronic product, communication apparatus, electric automobile, weaponry and aviation
The fields such as space flight.The fast development in each field also further proposes higher requirement to performance of lithium ion battery.Existing lithium
Ion battery positive electrode includes the LiMO of layer structure2, spinel structure LiM2O4With the LiMPO of olivine structural4（M=
The transition metal ions such as Co, Ni, Mn and V）With with stratiform ternary material, the lithium-rich manganese-based high-capacity material for representative.It is existing
Lithium ion battery negative material includes various carbon materials, tinbase, silicon substrate, titanate material and the oxo transition metal of industrialization
Compound etc..
The carbon material being widely used at present solves the safety issue of metal lithium electrode so that lithium ion battery
Commercialization is achieved.Carbon material includes graphitized carbon material and amorphous carbon material, such as native graphite, modified graphite, graphite
Change interphase, carbosphere, soft charcoal and some hard charcoals etc..The theoretical capacity of graphite carbon material is 372mAh/g, commercial applications
Carbon material capacity about in 330mAh/g.Although carbon material is had been achieved for larger entering for negative electrode of lithium ion battery
Exhibition, but be due to that its high-rate charge-discharge capability is poor, energy loss is serious, specific capacity irreversible loss is big and is easily caused
Forming Li dendrite causes the deficiencies such as short circuit to limit its further development.Tinbase, silica-base material have specific capacity high and electricity
Electrode potential is slightly higher compared with lithium to be avoided the advantage of Li dendrite generation and causes extensive research, but this kind of material is in discharge and recharge
During, experienced larger Volume Changes, electrode material can gradually efflorescence, cause battery capacity to decay rapidly.Titanate material
Material due to it in charge and discharge process the less feature of Volume Changes and be referred to as " zero strain material ".Such material is being used as lithium
During ion battery negative pole, there is stable discharge platform and good cycle performance.But the discharge platform of titanate is up to
1.55V so that the working voltage platform reduction of lithium ion battery, causes its application to be limited to.Transition metal oxide conduct
Lithium ion battery negative material can obtain considerable reversible capacity, but its cycle performance is poor, and reaction storage lithium mechanism also has
Treat in further research.Patoux and Masquelier have studied with α-VPO5The Li of structure2TiSiO5As lithium ion
The performance of battery electrode,（Referring to：Sebastien Patoux and Christian Masquelier. Lithium
Insertion into Titanium Phosphates, Silicates, and Sulfates. Chem Mater.
2002,14,5,057 5068,）They find the material without lithium ion insert and embedded performance, be not suitable for use in lithium from
Sub- battery electrode.
The content of the invention
The technical problems to be solved by the invention are to overcome the shortcomings of to mention with defect that there is provided one in background above technology
The novel cathode material for lithium ion battery with good performance of lithium ion battery is planted, a kind of raw material is correspondingly provided and is easy to get, operates
The preparation method of simple lithium ion battery negative material.
In order to solve the above technical problems, technical scheme proposed by the present invention is a kind of lithium ion battery negative material, it is changed
Formula is Li2TiSiO5, it is α-VPO5Structure, with three dimensions layer structure.Under room temperature condition, in 0.01~2.0V model
Constant current charge-discharge test is carried out with 10mA/g current density in enclosing, the reversible capacity for obtaining its charge and discharge process is more than
180mAh/g, the platform for taking off lithium process is 0.68~0.75V, and process of intercalation plateau potential is 0.28~0.35V.
As a total inventive concept, the present invention also provides a kind of preparation side of above-mentioned lithium ion battery negative material
Method, material is prepared using sol-gal process, specifically includes following steps：
（1）Titanium source and silicon source are dissolved in absolute ethyl alcohol, chelating agent is added, solution A is formed；
（2）Lithium salts is dissolved in the mixed solution of absolute ethyl alcohol and deionized water and forms solution B；
（3）Solution A is being slowly added in solution B during being stirred continuously to obtain leucosol, gained colloidal sol is being entered
Row heating water bath is simultaneously stirred, and obtains white gels；
（4）Above-mentioned white gels are placed in drying box and dried, presoma is obtained；
（5）After presoma is ground, pre-burning in Muffle furnace is placed in, then is calcined, the lithium ion battery negative material is obtained.
In above-mentioned preparation method, it is preferred that the elemental mole ratios of the lithium salts, titanium source and silicon source are Li:Ti:Si=
（2.00~2.25）:（0.95~1.05）:（0.95~1.05）.
In above-mentioned preparation method, it is preferred that the titanium source is butyl titanate, tetraethyl titanate, titanium tetraisopropylate, titanium
Any one in sour four isopropyl esters, tetrabutyl titanate amine；The silicon source is tetraethyl orthosilicate, methyl silicate, methyl three
Any one in Ethoxysilane.
In above-mentioned preparation method, it is preferred that the lithium salts is lithium chloride, lithium oxalate, lithium nitrate, lithium acetate or lithium sulfate
In any one.
In above-mentioned preparation method, it is preferred that the chelating agent is one kind or several in triethanolamine, oxalic acid or citric acid
Plant mixture.
In above-mentioned preparation method, it is preferred that the temperature of the heating water bath is 30~60 DEG C, the time of the stirring is
20~40h.
In above-mentioned preparation method, it is preferred that the temperature of the drying is 75~85 DEG C, the time is 16~24h.
In above-mentioned preparation method, it is preferred that the temperature of the pre-burning is 450~700 DEG C, the time is 3~5h；The roasting
The temperature of burning is 750~950 DEG C, and the time is 10~24h.
The present invention prepares the novel cathode material for lithium ion battery using sol-gal process, and raw material used can be effective
It is distributed in solvent, so as to form the solution of low viscosity.Various materials can obtain the equal of molecular level in a short period of time
Even property, realizes that molecular level Shangdi is uniformly mixed when forming gel.WithSolid phase reactionCompare, sol-gal process prepares material institute
The chemical reaction being related to will be carried out easily, and only need relatively low synthesis temperature, be conducive to controlling reaction condition, be obtained homogeneous
Product.
The present invention technique effect be：The present invention titanium silicate lithium material as lithium ion battery negative pole when, its discharge
Platform is in 0.3V（vs.Li+/Li）Left and right, hence it is evident that higher than the discharge platform 0.08V of graphite cathode material（vs.Li+/Li）, therefore
It is possible to prevente effectively from negative pole analyses lithium problem caused by polarization, it can greatly improve the security performance of battery；Than putting for lithium titanate
Level platform 1.55V（vs.Li+/Li）Low, initial charge specific capacity is more than 180mAh/g, hence it is evident that higher than lithium titanate specific capacity
160mAh/g, therefore relative to lithium ion battery of the lithium titanate as negative pole is used, use its charging/discharging voltage during titanium silicate lithium
Wider range, capacity is high, and the energy density of battery is highly improved, and cycle performance of battery is excellent.Material produced by the present invention
Material is with more gentle charge and discharge platform.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are the present invention
Some embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
These accompanying drawings obtain other accompanying drawings.
Fig. 1 is the charging and discharging curve figure of lithium ion battery negative material prepared by the embodiment of the present invention 1.
Fig. 2 is the loop test figure of lithium ion battery negative material prepared by the embodiment of the present invention 1.
Fig. 3 is the X-ray diffractogram of lithium ion battery negative material prepared by the embodiment of the present invention 1.
Embodiment
For the ease of understanding the present invention, more complete is made to the present invention below in conjunction with Figure of description and preferred embodiment
Face, meticulously describe, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, the implication that all technical terms used hereinafter are generally understood that with those skilled in the art
It is identical.Technical term used herein is intended merely to describe the purpose of specific embodiment, is not intended to the limitation present invention
Protection domain.
Unless otherwise specified, various raw material, reagent, instrument and equipment used in the present invention etc. can be by city
Field is commercially available or can prepared by existing method.
Embodiment 1：
A kind of lithium ion battery negative material of the invention, its chemical formula is Li2TiSiO5, the reversible appearance of charge and discharge process
Amount is more than 180mAh/g, and the platform for taking off lithium process is 0.68V, and the platform of process of intercalation is 0.35V, and charging/discharging voltage scope is
0.01~2.0V, initial charge specific capacity is 211.2mAh/g.
A kind of preparation method of the lithium ion battery negative material of the present embodiment, comprises the following steps：Weigh 8.1790g's
Butyl titanate and 5.053g tetraethyl orthosilicate are dissolved in 200ml ethanol, and the triethanolamine for adding 3.5138g forms molten
Liquid A.The lithium acetate for weighing 4.9998g is dissolved in the mixed solution of 100ml ethanol and 5ml water and forms solution B.It is being stirred continuously
During A is slowly added to B mixed solution, obtain leucosol, continue to stir,（Stirred in 30 DEG C of water-baths
20h）Colloidal sol is gradually become after white gels, and 16h is dried in 80 DEG C of drying box, obtains white xerogel presoma.Through
After grinding, presoma is placed in 450 DEG C of pre-burning 5h in Muffle furnace, 10h is calcined at 950 DEG C, obtain the lithium of the present embodiment from
Sub- cell negative electrode material.
By above-mentioned lithium ion battery negative material（Titanium silicate lithium）With conductive black, Kynoar（PVDF）With quality
Than 8:1:1 ground and mixed is uniform, adds appropriate 1-METHYLPYRROLIDONE（NMP）Pulpous state is tuned into, is coated on copper foil 120
DEG C drying box in dry 4h, be then cut into piece, anode plate for lithium ionic cell be made.Lithium ion battery obtained above is born
Pole pole piece is assembled into button cell and tests its performance.Its embedding lithium platform is in 0.35V, and initial charge specific capacity is 211.2mAh/g,
Charging and discharging curve as shown in figure 1,（As shown in Figure 1, by Li2TiSiO5During as lithium ion battery negative material, the material has
Relatively low charge and discharge platform and higher reversible capacity, are conducive to expanding the working voltage platform of lithium ion battery, with higher
Battery capacity.）Loop test curve is as shown in Figure 2.（As shown in Figure 2, by Li2TiSiO5It is used as lithium ion battery negative material
When, the capability retention of battery is good, is conducive to being lifted the service life of lithium ion battery.）X-ray diffractogram is as shown in Figure 3.
（By being contrasted with standard PDF cards, the PDF cards numbering obtained corresponding thereto is：97-007-8059.It can determine that
Li2TiSiO5With α-VPO5Structure, belongs to P4/nmm space groups.）
Embodiment 2：
A kind of lithium ion battery negative material of the invention, its chemical formula is Li2TiSiO5, the reversible appearance of charge and discharge process
Amount is more than 180mAh/g, and the platform for taking off lithium process is 0.72V, and the platform of process of intercalation is 0.28V, and charging/discharging voltage scope is
0.01~2.0V, initial charge specific capacity is 215.6mAh/g.
A kind of preparation method of the lithium ion battery negative material of the present embodiment, comprises the following steps：Weigh 5.4823g's
Tetraethyl titanate and 3.7305g methyl silicate are dissolved in 200ml ethanol, add 1.8851g oxalic acid formation solution A.
The lithium nitrate for weighing 1.6571g is dissolved in the mixed solution of 100ml ethanol and 5ml water and forms solution B.In the mistake being stirred continuously
A is slowly added to B mixed solution in journey, leucosol is obtained, continues to stir,（40h is stirred in 50 DEG C of water-baths）It is molten
Glue is gradually become after white gels, and 24h is dried in 85 DEG C of drying box, obtains white xerogel presoma.It is polished,
Presoma is placed in 700 DEG C of pre-burning 3h in Muffle furnace, 24h is calcined at 750 DEG C, the lithium ion battery for obtaining the present embodiment is born
Pole material.
By above-mentioned lithium ion battery negative material（Titanium silicate lithium）With conductive black, Kynoar（PVDF）With quality
Than 8:1:1 ground and mixed is uniform, adds appropriate 1-METHYLPYRROLIDONE（NMP）Pulpous state is tuned into, is coated on copper foil 120
DEG C drying box in dry 4h, be then cut into piece, anode plate for lithium ionic cell be made.Lithium ion battery obtained above is born
Pole pole piece is assembled into button cell and tests its performance.Its embedding lithium platform is in 0.28V, and initial charge specific capacity is 215.6mAh/g.
Embodiment 3：
A kind of lithium ion battery negative material of the invention, its chemical formula is Li2TiSiO5, the reversible appearance of charge and discharge process
Amount is more than 180mAh/g, and the platform for taking off lithium process is 0.75V, and the platform of process of intercalation is 0.32V, and charging/discharging voltage scope is
0.01~2.0V, initial charge specific capacity is 207.8mAh/g.
A kind of preparation method of the lithium ion battery negative material of the present embodiment, comprises the following steps：Weigh 6.8308g's
Titanium tetraisopropylate and 0.3294g MTES are dissolved in 200ml ethanol, add 2.078g triethanolamine shape
Into solution A.The lithium oxalate for weighing 4.3451g is dissolved in the mixed solution of 100ml ethanol and 5ml water and forms solution B.Continuous
A is slowly added to B mixed solution during stirring, leucosol is obtained.Continue to stir,（Stirred in 60 DEG C of water-baths
Mix 30h）Colloidal sol is gradually become after white gels, and 20h is dried in 75 DEG C of drying box, obtains white xerogel presoma.
It is polished, presoma is placed in 550 DEG C of pre-burning 4h in Muffle furnace, 20h is calcined at 870 DEG C, the lithium of the present embodiment is obtained
Ion battery cathode material.
By above-mentioned lithium ion battery negative material（Titanium silicate lithium）With conductive black, Kynoar（PVDF）With quality
Than 8:1:1 ground and mixed is uniform, adds appropriate 1-METHYLPYRROLIDONE（NMP）Pulpous state is tuned into, is coated on copper foil 120
DEG C drying box in dry 4h, be then cut into piece, anode plate for lithium ionic cell be made.Lithium ion battery obtained above is born
Pole pole piece is assembled into button cell and tests its performance.Its embedding lithium platform is in 0.32V, and initial charge specific capacity is 207.8mAh/g.
Claims (7)
1. a kind of preparation method of lithium ion battery negative material, it is characterised in that material is prepared using sol-gal process, specifically
Comprise the following steps：
（1）Titanium source and silicon source are dissolved in absolute ethyl alcohol, chelating agent is added, solution A is formed；
（2）Lithium salts is dissolved in the mixed solution of absolute ethyl alcohol and deionized water and forms solution B；
（3）Solution A is being slowly added in solution B during being stirred continuously to obtain leucosol, gained colloidal sol is entered into water-filling
Bath is heated and stirred, and obtains white gels；
（4）Above-mentioned white gels are placed in drying box and dried, presoma is obtained；
（5）After presoma is ground, pre-burning in Muffle furnace is placed in, then is calcined, the lithium ion battery negative material is obtained；
The temperature of the pre-burning is 450~700 DEG C, and the time is 3~5h；The temperature of the roasting is 750~950 DEG C, and the time is
10~24h；
Described lithium ion battery negative material, its chemical formula is Li2TiSiO5, it is α-VPO5Structure, with three dimensions stratiform
Structure；Under room temperature condition, constant current charge-discharge test is carried out with 10mA/g current density in the range of 0.01~2.0V, obtained
Reversible capacity to its charge and discharge process is more than 180mAh/g, and the platform for taking off lithium process is 0.68~0.75V, process of intercalation
Platform is 0.28~0.35V.
2. preparation method according to claim 1, it is characterised in that the elemental mole ratios of the lithium salts, titanium source and silicon source
For Li:Ti:Si=2.00~2.25:0.95~1.05:0.95~1.05.
3. preparation method according to claim 1, it is characterised in that the titanium source be butyl titanate, tetraethyl titanate,
Any one in titanium tetraisopropylate, tetraisopropyl titanate, tetrabutyl titanate amine；The silicon source is tetraethyl orthosilicate, positive silicon
Any one in sour methyl esters, MTES.
4. preparation method according to claim 1, it is characterised in that the lithium salts be lithium chloride, lithium oxalate, lithium nitrate,
Any one in lithium acetate or lithium sulfate.
5. preparation method according to claim 1, it is characterised in that the chelating agent is triethanolamine, oxalic acid or lemon
One or more of mixtures in acid.
6. preparation method according to claim 1, it is characterised in that the temperature of the heating water bath is 30~60 DEG C, institute
The time for stating stirring is 20~40h.
7. the preparation method according to any one of claim 1 ~ 6, it is characterised in that the temperature of the drying is 75~85
DEG C, the time is 16~24h.
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| CN105140516B (en) * | 2015-09-10 | 2017-11-21 | 中南大学 | A kind of method that titanium silicate lithium titanate cathode material is prepared using ilmenite |
| CN105226281A (en) * | 2015-10-20 | 2016-01-06 | 复旦大学 | The titanium silicate lithium titanate cathode material of lithium ion battery and preparation method and application |
| CN109950502B (en) * | 2019-04-01 | 2020-11-27 | 北京工业大学 | TiO 22Preparation method and application of domain structure regulated titanium lithium silicate material |
| CN114014330B (en) * | 2021-11-03 | 2024-09-24 | 蚌埠学院 | Energy storage electrode material K3Nb3Si2O13Preparation method and application of (C) |
| CN113998705B (en) * | 2021-11-03 | 2024-08-06 | 蚌埠学院 | Ba (Bay)3Nb6Si4O26Preparation method and application of lithium ion battery anode material |
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| CN102623698A (en) * | 2012-04-16 | 2012-08-01 | 南京大学 | Titanium lithium silicate, preparation method thereof and use of the same serving as electrode material of lithium battery |
| CN103545502A (en) * | 2013-10-30 | 2014-01-29 | 合肥恒能新能源科技有限公司 | Compound element-doped modified lithium titanate anode material and preparation method thereof |
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