CN106972170A - A kind of lithium titanate electrode material with composite pore structural and preparation method thereof - Google Patents
A kind of lithium titanate electrode material with composite pore structural and preparation method thereof Download PDFInfo
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- CN106972170A CN106972170A CN201710387580.8A CN201710387580A CN106972170A CN 106972170 A CN106972170 A CN 106972170A CN 201710387580 A CN201710387580 A CN 201710387580A CN 106972170 A CN106972170 A CN 106972170A
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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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- 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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- 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 belongs to electrode material technical field, and in particular to a kind of lithium titanate electrode material with composite pore structural and preparation method thereof.This method prepares the titanium dioxide with composite pore structural in the method for double template system first, then prepares the material by solid-phase synthesis with lithium source.The lithium titanate electrode material with composite pore structural that the inventive method is prepared, first charge-discharge specific capacity is 173.4mAh/g, is the 99.1% of lithium titanate material theoretical specific capacity, its tap density is up to 1.05 1.15g/cm3.
Description
Technical field
The invention belongs to electrode material technical field, and in particular to a kind of lithium titanate electrode material with composite pore structural
And preparation method thereof.
Background technology
Compared with commercialized lithium ion battery negative pole carbon material, the lithium titanate Li4Ti5O12 of spinel structure, which has, to be stood
Square structure and " zero strain " performance, with good dynamic performance and stability；The activity reacted with electrolyte is smaller, is difficult
Form impedance layer；High-specific surface area, the dynamics with quick charge；Without the generation of SEI films, with good heat endurance
The advantages of with security feature.But the material has relatively low electrical conductivity (about 10-9S/cm) in itself, in charge and discharge process
The internal resistance of cell and resistance to mass tranfer can substantially be increased, larger polarization is produced, increase energy loss, high power charging-discharging is reduced
Energy.
In view of the problem of above lithium titanate material is present, researcher's majority enters in terms of the electric conductivity of the material is improved
One step improves the high rate performance of material, the even nano level lithium titanate of fine particle size is such as used, to shorten the migration of lithium ion
Path, improves high rate performance；Electrical conductivity is also improved using carbon coated or doping metals powder or its oxide, is improved again
Rate characteristic etc..And this technology solution is further to improve final products lithium titanate by changing the structure of lithium titanate material
Overall performance, currently without finding the patented method for preparing lithium titanate close with this technology solution.
The content of the invention
It is an object of the invention to solve above-mentioned technical problem there is provided a kind of tap density height, with composite pore structural point
Lithium titanate material that cloth, the conductance of material and high rate performance are improved and preparation method thereof.
To achieve the above object, the technical solution adopted in the present invention is：
A kind of preparation method of the lithium titanate electrode material with composite pore structural, comprises the following steps：
(1) tetraethyl ammonium hydroxide solution, ammoniacal liquor are well mixed with water, wherein tetraethyl ammonium hydroxide solution, ammoniacal liquor
Volume ratio with water is 1:3-5:10-15；
(2) then be added dropwise titanyl sulfate solution, stir 3-6 hour, add polyvinyl alcohol, continue stirring 4-8 hours, its
In, the volume ratio of titanyl sulfate solution and tetraethyl ammonium hydroxide is 12-14:1, the body of polyvinyl alcohol and tetraethyl ammonium hydroxide
Product is than being 0.8-1.2:1；
(3) above-mentioned solution is loaded into reactor, after standing 6-8 hours under conditions of 100-120 DEG C, is cooled to room temperature,
Filtering, with absolute ethyl alcohol washing precipitate untill sulfate radical-free, drying is calcined 3-5 hours at 420-550 DEG C, is cooled to
Room temperature, obtains the titanium dioxide powder with composite pore structural；
(4) Li is pressed：Ti mol ratios weigh lithium salts and titanium dioxide in ball mill container for 0.8-0.86 ratio, add and divide
Powder carries out ball milling, is then calcined, and 4-6 hours are incubated at 500-600 DEG C, then heats to 700-800 DEG C, is incubated 8-
12 hours, room temperature is cooled to, the described lithium titanate electrode material with composite pore structural is produced.
Further, the dispersant is absolute ethyl alcohol or acetone, and it accounts for the 5-20% of titanium dioxide and lithium salts gross mass.
Further, the lithium salts is the one or more in lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate, lithium oxalate
Mixing.
Further, the Ball-milling Time is 2-4 hours.
A kind of lithium titanate electrode material with composite pore structural, is prepared by the above method.
The present invention has the advantages and positive effects of：
(1) lithium titanate electrode material with composite pore structural that the inventive method is prepared, first charge-discharge specific volume
Amount is 173.4mAh/g, is the 99.1% of lithium titanate material theoretical specific capacity.This is due to the composite pore structural of lithium titanate material,
Be conducive to fully contacting for active material and electrolyte, the more transmission due to lithium ion between active material and electrolyte, big
Polarization resistance caused by being also easy to produce activation polarization and concentration polarization is not allowed to improve during current discharge so that with composite holes knot
Specific capacity can preferably be brought into play during the lithium titanate electrode material discharge and recharge of structure.
(2) preparation method of the invention is by using tetraethyl ammonium hydroxide and polyvinyl alcohol as template, being oriented to synthesis tool
There is the titanium dioxide of composite pore structural, make material of the present invention that there is abundant pore structure, substantially increase the specific surface area of material,
Reduce diffusion length of the lithium ion in lithium titanate.
(3) due to pore structure that titanium dioxide is combined in itself, it is to avoid in calcination process due to solvent evaporation and
Big hole is formed in lithium titanate material body, the tap density of material after sintering is improved, its tap density is up to 1.05-
1.15g/cm3。
Embodiment
The present invention is specifically described and illustrated below by embodiment：
Embodiment 1
A kind of lithium titanate electrode material with composite pore structural, its preparation method comprises the following steps：
(1) tetraethyl ammonium hydroxide solution, ammoniacal liquor are well mixed with water, wherein tetraethyl ammonium hydroxide solution, ammoniacal liquor
Volume ratio with water is 1:5:10；
(2) then be added dropwise titanyl sulfate solution, stir 6 hours, add polyvinyl alcohol, continue stir 4 hours, wherein, sulphur
The volume ratio of sour oxygen titanium solution and tetraethyl ammonium hydroxide is 14:1, the volume ratio of polyvinyl alcohol and tetraethyl ammonium hydroxide is
0.8:1；
(3) above-mentioned solution is loaded into reactor, after standing 6 hours under conditions of 120 DEG C, is cooled to room temperature, filters, use
Absolute ethyl alcohol washing precipitate is untill sulfate radical-free, and drying is calcined 3 hours at 550 DEG C, is cooled to room temperature, is obtained with multiple
Close the titanium dioxide powder of pore structure；
(4) Li is pressed：Ti mol ratios weigh lithium salts and titanium dioxide in ball mill container for 0.86 ratio, and the lithium salts is
One or more mixing in lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate, lithium oxalate, add dispersant progress ball milling 2 small
When, dispersant is absolute ethyl alcohol or acetone, and it accounts for the 20% of titanium dioxide and lithium salts gross mass, then calcined, at 500 DEG C
Lower insulation 6 hours, then heats to 700 DEG C, is incubated 12 hours, is cooled to room temperature, and producing described has composite pore structural
Lithium titanate electrode material.Its tap density is 1.15g/cm3。
Lithium ion battery is prepared using lithium titanate material made from the present embodiment as active material.With 1-METHYLPYRROLIDONE
(NMP) it is solvent, by lithium titanate material made from the present embodiment and conductive agent acetylene black and binding agent Kynoar
(PVDF) in mass ratio 8: 1: 1 be uniformly mixed after prepare slurry, be then coated on Al paper tinsels, be cold-pressed and be washed into after drying
The sequin of 14mm diameters.Using obtained sequin as negative electrode, metal lithium sheet is to electrode, the micropores of Celgard 2400 poly- third
Alkene film is barrier film, and 1M LiPF6/ (EC+DEC) (1: 1, volume ratio) solution is assembled into 2032 button half-cells for electrolyte.
Cyclic voltammetry and constant current charge-discharge test are then carried out, as a result first discharge specific capacity reaches 170mAh/g,
The chemical property of material is substantially undamped after being circulated 500 times under 1C multiplying powers, and stability is preferable.
Embodiment 2
A kind of lithium titanate electrode material with composite pore structural, its preparation method comprises the following steps：
(1) tetraethyl ammonium hydroxide solution, ammoniacal liquor are well mixed with water, wherein tetraethyl ammonium hydroxide solution, ammoniacal liquor
Volume ratio with water is 1:3:15；
(2) then be added dropwise titanyl sulfate solution, stir 3 hours, add polyvinyl alcohol, continue stir 8 hours, wherein, sulphur
The volume ratio of sour oxygen titanium solution and tetraethyl ammonium hydroxide is 12:1, the volume ratio of polyvinyl alcohol and tetraethyl ammonium hydroxide is
1.2:1；
(3) above-mentioned solution is loaded into reactor, after standing 8 hours under conditions of 100 DEG C, is cooled to room temperature, filters, use
Absolute ethyl alcohol washing precipitate is untill sulfate radical-free, and drying is calcined 5 hours at 420 DEG C, is cooled to room temperature, is obtained with multiple
Close the titanium dioxide powder of pore structure；
(4) Li is pressed：Ti mol ratios weigh lithium salts and titanium dioxide in ball mill container for 0.8 ratio, and the lithium salts is
One or more mixing in lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate, lithium oxalate, add dispersant progress ball milling 4 small
When, dispersant is absolute ethyl alcohol or acetone, and it accounts for the 5% of titanium dioxide and lithium salts gross mass, then calcined, at 600 DEG C
Lower insulation 4 hours, then heats to 800 DEG C, is incubated 8 hours, is cooled to room temperature, produces the described titanium with composite pore structural
Sour lithium electrode material.Its tap density is 1.07g/cm3。
Lithium ion battery is prepared using lithium titanate material made from the present embodiment as active material.With 1-METHYLPYRROLIDONE
(NMP) it is solvent, by lithium titanate material made from the present embodiment and conductive agent acetylene black and binding agent Kynoar
(PVDF) in mass ratio 8: 1: 1 be uniformly mixed after prepare slurry, be then coated on Al paper tinsels, be cold-pressed and be washed into after drying
The sequin of 14mm diameters.Using obtained sequin as negative electrode, metal lithium sheet is to electrode, the micropores of Celgard 2400 poly- third
Alkene film is barrier film, and 1M LiPF6/ (EC+DEC) (1: 1, volume ratio) solution is assembled into 2032 button half-cells for electrolyte.
Cyclic voltammetry and constant current charge-discharge test are then carried out, as a result first discharge specific capacity reaches 171mAh/g,
The chemical property of material is substantially undamped after being circulated 500 times under 1C multiplying powers, and stability is preferable.
Embodiment 3
A kind of lithium titanate electrode material with composite pore structural, its preparation method comprises the following steps：
(1) tetraethyl ammonium hydroxide solution, ammoniacal liquor are well mixed with water, wherein tetraethyl ammonium hydroxide solution, ammoniacal liquor
Volume ratio with water is 1:4:12；
(2) then be added dropwise titanyl sulfate solution, stir 5 hours, add polyvinyl alcohol, continue stir 6 hours, wherein, sulphur
The volume ratio of sour oxygen titanium solution and tetraethyl ammonium hydroxide is 13:1, the volume ratio of polyvinyl alcohol and tetraethyl ammonium hydroxide is 1:
1；
(3) above-mentioned solution is loaded into reactor, after standing 7 hours under conditions of 110 DEG C, is cooled to room temperature, filters, use
Absolute ethyl alcohol washing precipitate is untill sulfate radical-free, and drying is calcined 4 hours at 500 DEG C, is cooled to room temperature, is obtained with multiple
Close the titanium dioxide powder of pore structure；
(4) Li is pressed：Ti mol ratios weigh lithium salts and titanium dioxide in ball mill container for 0.83 ratio, and the lithium salts is
One or more mixing in lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate, lithium oxalate, add dispersant progress ball milling 3 small
When, dispersant is absolute ethyl alcohol or acetone, and it accounts for the 15% of titanium dioxide and lithium salts gross mass, then calcined, at 550 DEG C
Lower insulation 5 hours, then heats to 750 DEG C, is incubated 10 hours, is cooled to room temperature, and producing described has composite pore structural
Lithium titanate electrode material.Its tap density is 1.12g/cm3。
Lithium ion battery is prepared using lithium titanate material made from the present embodiment as active material.With 1-METHYLPYRROLIDONE
(NMP) it is solvent, by lithium titanate material made from the present embodiment and conductive agent acetylene black and binding agent Kynoar
(PVDF) in mass ratio 8: 1: 1 be uniformly mixed after prepare slurry, be then coated on Al paper tinsels, be cold-pressed and be washed into after drying
The sequin of 14mm diameters.Using obtained sequin as negative electrode, metal lithium sheet is to electrode, the micropores of Celgard 2400 poly- third
Alkene film is barrier film, and 1M LiPF6/ (EC+DEC) (1: 1, volume ratio) solution is assembled into 2032 button half-cells for electrolyte.
Cyclic voltammetry and constant current charge-discharge test are then carried out, as a result first discharge specific capacity reaches 171mAh/g,
The chemical property of material is substantially undamped after being circulated 500 times under 1C multiplying powers, and stability is preferable.
Comparative example 1
By Li：Ti mol ratios weigh lithium salts and titanium dioxide in ball mill container for 0.83 ratio, and the lithium salts is carbon
One or more mixing in sour lithium, lithium hydroxide, lithium nitrate, lithium acetate, lithium oxalate, add dispersant and carry out ball milling 3 hours,
Dispersant is absolute ethyl alcohol or acetone, and it accounts for the 15% of titanium dioxide and lithium salts gross mass, then calcined, at 550 DEG C
Insulation 5 hours, then heats to 750 DEG C, is incubated 10 hours, is cooled to room temperature, produces common lithium titanate electrode material.Its jolt ramming
Density is 0.87g/cm3。
Lithium ion battery is prepared using lithium titanate material made from this comparative example as active material.Preparation method be the same as Example 1.
Cyclic voltammetry and constant current charge-discharge test are then carried out, as a result first discharge specific capacity reaches 150mAh/g,
The capability retention of material is 75% after being circulated 500 times under 1C multiplying powers.
Here is the BET characterization results of products obtained therefrom of the present invention：
The BET characterization results of the embodiment of the present invention of table 1 and comparative example
The specific surface area and pore volume that can be seen that the material that the inventive method is prepared from the data in table 1 are substantially high
In the sample of comparative example, from the point of view of mesopore surface area and micropore specific area distribution, it was demonstrated that in the lithium titanate material of the present invention
With compound mesoporous-microcellular structure.
Claims (5)
1. a kind of preparation method of the lithium titanate electrode material with composite pore structural, it is characterised in that comprise the following steps：
（1）Tetraethyl ammonium hydroxide solution, ammoniacal liquor are well mixed with water, wherein tetraethyl ammonium hydroxide solution, ammoniacal liquor and water
Volume ratio be 1:3-5:10-15；
（2）Then titanyl sulfate solution is added dropwise, stirs 3-6 hours, polyvinyl alcohol is added, continues to stir 4-8 hours, wherein, sulphur
The volume ratio of sour oxygen titanium solution and tetraethyl ammonium hydroxide is 12-14:1, the volume ratio of polyvinyl alcohol and tetraethyl ammonium hydroxide
For 0.8-1.2:1；
（3）Above-mentioned solution is loaded into reactor, after standing 6-8 hours under conditions of 100-120 DEG C, room temperature is cooled to, filters,
With absolute ethyl alcohol washing precipitate untill sulfate radical-free, drying is calcined 3-5 hours at 420-550 DEG C, is cooled to room temperature,
There must be the titanium dioxide powder of composite pore structural；
（4）By Li：Ti mol ratios weigh lithium salts and titanium dioxide in ball mill container for 0.8-0.86 ratio, add dispersant
Ball milling is carried out, is then calcined, 4-6 hours are incubated at 500-600 DEG C, 700-800 DEG C is then heated to, insulation 8-12 is small
When, room temperature is cooled to, the described lithium titanate electrode material with composite pore structural is produced.
2. preparation method according to claim 1, it is characterised in that the dispersant is absolute ethyl alcohol or acetone, and it is accounted for
The 5-20% of titanium dioxide and lithium salts gross mass.
3. preparation method according to claim 1, it is characterised in that the lithium salts is lithium carbonate, lithium hydroxide, nitric acid
One or more mixing in lithium, lithium acetate, lithium oxalate.
4. preparation method according to claim 1, it is characterised in that the Ball-milling Time is 2-4 hours.
5. a kind of lithium titanate electrode material with composite pore structural, it is characterised in that by described in claim any one of 1-4
Method is prepared.
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