CN108520953A - A kind of carbon coating lithium titanate negative material and preparation method thereof - Google Patents
A kind of carbon coating lithium titanate negative material and preparation method thereof Download PDFInfo
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- CN108520953A CN108520953A CN201810342297.8A CN201810342297A CN108520953A CN 108520953 A CN108520953 A CN 108520953A CN 201810342297 A CN201810342297 A CN 201810342297A CN 108520953 A CN108520953 A CN 108520953A
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
A kind of carbon coating lithium titanate negative material and preparation method thereof, belongs to electrode material of lithium battery preparing technical field.The present invention first synthesizes lithium titanate, is then uniformly mixed with cysteine, is roasted under inert atmosphere protection and obtains carbon-coated lithium titanate anode material.The present invention improves electric conductivity by cladding nitrogen, the carbon of sulfur doping, assigns lithium titanate material more excellent circulating ratio performance and electrochemical stability.Gained lithium titanate anode material pattern is irregular polyhedrons particle, and surface has coated the carbon-coating of nitrogen, sulphur codope, and relative to pure lithium titanate, high rate performance and cyclical stability are increased substantially.Experiment shows that carbon coating lithium titanate specific capacity is 170mAh g under 0.2C multiplying powers‑1Left and right, and lithium titanate specific capacity is in 140mAh g‑1Left and right；With the increase of multiplying power, the specific capacity of carbon coating lithium titanate is higher than lithium titanate.
Description
Technical field
The invention belongs to electrode material of lithium battery preparing technical fields, and in particular to a kind of carbon coating lithium titanate negative material
And preparation method thereof.
Background technology
With energy crisis and increasingly prominent environmental problem, new green power becomes research hotspot.Lithium ion battery
With the advantages of long lifespan, energy density is high, memory-less effect, in mancarried electronic aid, electric vehicle, large-scale energy-accumulating power station etc.
Field has a wide range of applications.
Spinel lithium titanate (Li4Ti5O12) as lithium ion battery negative material of new generation, there is lithium ion deintercalation structure
Zero strain, intercalation potential height (1.55V vs Li/Li+), discharge voltage plateau is steady, and cyclical stability is excellent, the spies such as safety height
Point.But lithium titanate is a kind of material almost to insulate, electron conduction is poor, and ionic conductivity is not high, causes its high power forthright
It can be poor.Currently, common method of modifying has body phase element doping, crystallite dimension, the methods of coating conducting substance are controlled.
In order to improve the high rate capability of lithium titanate anode material, present invention cysteine and lithium titanate are baking mixed,
Obtain the lithium titanate anode material of the conductive carbon of surface cladding nitrogen, sulphur codope.
Invention content
Low it is an object of the invention to be directed to lithium titanate conductivity present in current techniques, high rate capability difference lacks
Point provides a kind of carbon coating lithium titanate negative material and preparation method thereof.Lithium cell cathode material prepared by this method has height
The features such as good rate capability, good cycle, efficiency for charge-discharge is high.
A kind of preparation method of carbon coating lithium titanate negative material of the present invention, its step are as follows：
(1) lithium compound and titanium compound are added in absolute ethyl alcohol, be stirred at room temperature (100~300rpm) 8~
24h；
(2) deionized water is added under strong stirring (400~1000rpm) in the solution that step (1) obtains, and is further continued for stirring
1~30min；
(3) liquid for obtaining step (2) 24~48h of hydro-thermal reaction at 140~220 DEG C is cooled to after the completion of reaction
Room temperature is centrifuged solid product, absolute ethyl alcohol washs, dry；
(4) product that step (3) obtains is roasted in air and obtains lithium titanate；
(5) lithium titanate that step (4) obtains is uniformly mixed with cysteine, is roasted in protective atmosphere and obtains the present invention
The carbon coating lithium titanate negative material.
In step (1), the lithium compound is in lithium hydroxide, lithium chloride, lithium acetate, lithium carbonate, lithium oxalate, lithia
One kind, preferably lithium hydroxide.
In step (1), the titanium compound is in butyl titanate, tetraethyl titanate, tetraisopropyl titanate, titanyl sulfate
One kind, preferably butyl titanate, tetraethyl titanate.
The molar ratio of lithium ion and titanium ion is 0.78~0.92 in step (1)：1, the concentration of lithium ion in absolute ethyl alcohol
For 0.16~0.2mol L-1。
In step (2), the volume ratio of deionized water and absolute ethyl alcohol is 1~1.25：1.
It is in 60~90 DEG C of air dryings 4~for 24 hours in step (3).
The calcination temperature of step (4) is 500~700 DEG C, and roasting time is 5~7h, and roasting heating rate is 2~20 DEG C
min-1。
The lithium titanate of step (5) and the mass ratio of cysteine are 1~5：1.
The protective atmosphere of step (5) is one kind in argon gas, nitrogen, argon-hydrogen gaseous mixture, nitrogen-hydrogen gaseous mixture.
The calcination temperature of step (5) is 500~700 DEG C, and roasting time is 2~8h, and roasting heating rate is 2~10 DEG C
min-1, obtain carbon coating lithium titanate negative material of the present invention.
A kind of carbon coating lithium titanate negative material of the present invention, is prepared by the above method.
The advantage of the invention is that：By coating the carbon of nitrogen, sulfur doping, electric conductivity is improved, assigns lithium titanate material more
Add excellent circulating ratio performance and electrochemical stability.Gained lithium titanate anode material pattern is irregular polyhedrons particle,
Surface has coated the carbon-coating of nitrogen, sulphur codope, and relative to pure lithium titanate, high rate performance and cyclical stability have obtained significantly carrying
It is high.
Description of the drawings
Fig. 1：The embodiment of the present invention 1 prepare carbon coating lithium titanate X-ray diffraction (XRD) spectrogram, product peak position with
Standard spectrogram PDF#49-0207 is completely corresponding, illustrates that the sample that the present invention synthesizes is lithium titanate pure phase.
Fig. 2：The pattern of the SEM figures of carbon coating lithium titanate prepared by the embodiment of the present invention 2, sample is irregular polyhedrons grain
Son.
Fig. 3：The charge-discharge magnification comparison diagram of carbon coating lithium titanate and lithium titanate prepared by the embodiment of the present invention 1,0.2C times
Carbon coating lithium titanate specific capacity is 170mAh g under rate-1Left and right, and lithium titanate specific capacity is in 140mAh g-1Left and right；With multiplying power
Increase, the specific capacity of carbon coating lithium titanate is higher than lithium titanate, and multiplying power is finally set back 0.2C, the specific volume of carbon coating lithium titanate
Amount is still 170mAh g-1Left and right, and it is higher than lithium titanate.Illustrate that carbon coating lithium titanate is forthright with more superior than pure lithium titanate times
Matter.
Fig. 4：The cycle performance curve of carbon coating lithium titanate prepared by the embodiment of the present invention 5 under 1C multiplying powers, carbon coating titanium
Sour lithium continuously recycles 100 times under 1C multiplying powers, and capacitance loss rate illustrates that carbon coating lithium titanate has excellent electrification less than 5%
Learn stability.
Specific implementation mode
In conjunction with following instance, the present invention is further explained, but not only limits these examples.
Embodiment 1
(1) 0.212g lithium hydroxides are weighed to be added in 30mL absolute ethyl alcohols, 10min is stirred at room temperature, measure 2.1mL
Butyl titanate is added in above-mentioned solution, and (300rpm) 15h is stirred at room temperature；
(2) solution that step (1) obtains is under strong stirring state (500rpm), and 35mL deionized waters, stirring is added
3min；
(3) liquid for obtaining step (2) hydro-thermal reaction 35h at 180 DEG C；It is cooled to room temperature, will consolidate after the completion of reaction
Body product is centrifuged, absolute ethyl alcohol washing is multiple, then in 80 DEG C of air drying 10h；
(4) product for obtaining step (3) roasts 5.5h for 600 DEG C in air, obtains lithium titanate；
(5) lithium titanate for obtaining step (4) and cysteine are with mass ratio 2.5:1 is uniformly mixed, in nitrogen atmosphere
In tube furnace, 8h is roasted at 600 DEG C with the heating rate of 5 DEG C/min, obtains 0.394g carbon coating metatitanic acids of the present invention
Lithium titanate cathode material.
Embodiment 2
(1) 0.212g lithium hydroxides are weighed to be added in 30mL absolute ethyl alcohols, stir 30min, measure four fourth of 2.1mL metatitanic acids
Ester is added in above-mentioned solution, and (200rpm) 11h is stirred at room temperature；
(2) solution that step (1) obtains is under strong stirring state (600rpm), and 30mL deionized waters, stirring is added
30min；
(3) liquid for obtaining step (2) hydro-thermal reaction 36.5h at 180 DEG C；It is cooled to room temperature after the completion of reaction, it will
Solid product centrifuged, absolute ethyl alcohol washing is multiple, then 80 DEG C of air dryings for 24 hours；
(4) product for obtaining step (3) roasts 6.2h for 610 DEG C in air, obtains lithium titanate；
(5) lithium titanate for obtaining step (4) and cysteine are with mass ratio 5:1 is uniformly mixed, in the pipe of argon gas atmosphere
In formula stove, 3h is roasted at 600 DEG C with the heating rate of 10 DEG C/min, obtains 0.383g carbon coating lithium titanates of the present invention
Negative material.
Embodiment 3
(1) 2.68mL butyl titanates are measured to be added in 30mL absolute ethyl alcohols, stirs 5min, weighs 0.281g hydroxides
Lithium is added in above-mentioned solution, and (250rpm) 12.5h is stirred at room temperature；
(2) solution that step (1) obtains is under strong stirring state (800rpm), and 32mL deionized waters, stirring is added
1min；
(3) liquid for obtaining step (2) hydro-thermal reaction 36h at 180 DEG C；It is cooled to room temperature, will consolidate after the completion of reaction
Body product is centrifuged, absolute ethyl alcohol washing is multiple, then in 60 DEG C of air drying 5h；
(4) product for obtaining step (3) roasts 6.5h for 620 DEG C in air, obtains lithium titanate；
(5) lithium titanate for obtaining step (4) and cysteine are with mass ratio 4:1 is uniformly mixed, in argon gas and hydrogen (hydrogen
Gas fraction is to roast 4.5h at 600 DEG C with the heating rate of 3 DEG C/min, obtain 5%) in the tube furnace of mixed atmosphere
0.534g carbon coating lithium titanate negative materials of the present invention.
Embodiment 4
(1) 2.68mL butyl titanates are measured to be added in 35mL absolute ethyl alcohols, stirs 5min, weighs 0.281g hydroxides
Lithium is added in above-mentioned solution, and (200rpm) 20h is stirred at room temperature；
(2) solution that step (1) obtains is under strong stirring state (600rpm), and 40mL deionized waters, stirring is added
2min；
(3) liquid for obtaining step (2) hydro-thermal reaction 38h at 180 DEG C；It is cooled to room temperature, will consolidate after the completion of reaction
Body product is centrifuged, absolute ethyl alcohol washing is multiple, then in 70 DEG C of air drying 15.5h；
(4) product for obtaining step (3) roasts 6.5h for 590 DEG C in air, obtains lithium titanate；
(5) lithium titanate for obtaining step (4) and cysteine are with mass ratio 3.5:1 is uniformly mixed, in argon gas atmosphere
In tube furnace, 3.5h is roasted at 580 DEG C with the heating rate of 6 DEG C/min, obtains 0.541g carbon coating titaniums of the present invention
Sour lithium titanate cathode material.
Embodiment 5
(1) 2.68mL butyl titanates are measured to be added in 35mL absolute ethyl alcohols, stirs 1min, weighs 0.281g hydroxides
Lithium is added in above-mentioned solution, and (300rpm) 11.5h is stirred at room temperature；
(2) solution that step (1) obtains is under strong stirring state (600rpm), and 38mL deionized waters, stirring is added
1.5min；
(3) liquid for obtaining step (2) hydro-thermal reaction 35.5h at 180 DEG C；It is cooled to room temperature after the completion of reaction, it will
Solid product is centrifuged, absolute ethyl alcohol washing is multiple, then in 90 DEG C of air drying 8h；
(4) product for obtaining step (3) roasts 6.1h for 650 DEG C in air, obtains lithium titanate；
(5) lithium titanate for obtaining step (4) and cysteine are with mass ratio 3:1 is uniformly mixed, in nitrogen gas atmosphere
In tube furnace, 5h is roasted at 590 DEG C with the heating rate of 8 DEG C/min, obtains 0.527g carbon coating metatitanic acids of the present invention
Lithium titanate cathode material.
Claims (10)
1. a kind of preparation method of carbon coating lithium titanate negative material, its step are as follows：
(1) lithium compound and titanium compound are added in absolute ethyl alcohol, it is stirred at room temperature 8~for 24 hours；
(2) deionized water is added under strong stirring in the solution that step (1) obtains, and is further continued for 1~30min of stirring；
(3) liquid for obtaining step (2) 24~48h of hydro-thermal reaction at 140~220 DEG C is cooled to room temperature after the completion of reaction,
Solid product is centrifuged, absolute ethyl alcohol washs, dry；
(4) product that step (3) obtains is roasted in air and obtains lithium titanate；
(5) lithium titanate that step (4) obtains is uniformly mixed with cysteine, is roasted in protective atmosphere and obtains carbon coating metatitanic acid
Lithium titanate cathode material.
2. a kind of preparation method of carbon coating lithium titanate negative material as described in claim 1, it is characterised in that：Step (1)
Described in lithium compound be lithium hydroxide, lithium chloride, lithium acetate, lithium carbonate, lithium oxalate or lithia in one kind.
3. a kind of preparation method of carbon coating lithium titanate negative material as described in claim 1, it is characterised in that：Step (1)
Described in titanium compound be butyl titanate, tetraethyl titanate, tetraisopropyl titanate or titanyl sulfate in one kind.
4. a kind of preparation method of carbon coating lithium titanate negative material as described in claim 1, it is characterised in that：Step (1)
The molar ratio of middle lithium ion and titanium ion is 0.78~0.92：1, a concentration of 0.16~0.2mol of lithium ion in absolute ethyl alcohol
L-1。
5. a kind of preparation method of carbon coating lithium titanate negative material as described in claim 1, it is characterised in that：Step (2)
In, the volume ratio of deionized water and absolute ethyl alcohol is 1~1.25：1.
6. a kind of preparation method of carbon coating lithium titanate negative material as described in claim 1, it is characterised in that：Step (3)
In, it is in 60~90 DEG C of air dryings 4~for 24 hours.
7. a kind of preparation method of carbon coating lithium titanate negative material as described in claim 1, it is characterised in that：Step (4)
Calcination temperature be 500~700 DEG C, roasting time be 5~7h, roasting heating rate be 2~20 DEG C of min-1。
8. a kind of preparation method of carbon coating lithium titanate negative material as described in claim 1, it is characterised in that：Step (5)
Lithium titanate and cysteine mass ratio be 1~5：1；Protective atmosphere is argon gas, nitrogen, argon-hydrogen gaseous mixture or nitrogen-hydrogen mixing
One kind in gas.
9. a kind of preparation method of carbon coating lithium titanate negative material as described in claim 1, it is characterised in that：Step (5)
Calcination temperature be 500~700 DEG C, roasting time be 2~8h, roasting heating rate be 2~10 DEG C of min-1。
10. a kind of carbon coating lithium titanate negative material, it is characterised in that：It is by claim 1~9 any one of them method system
It is standby to obtain.
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Cited By (3)
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| CN110854375A (en) * | 2019-11-26 | 2020-02-28 | 石家庄昭文新能源科技有限公司 | Preparation method and application of Ti-MOF metal organic framework material, lithium titanate and carbon-coated lithium titanate |
| CN113258046A (en) * | 2021-05-19 | 2021-08-13 | 郑州航空工业管理学院 | Lithium/sodium ion battery negative electrode material and preparation method thereof |
| WO2024124961A1 (en) * | 2022-12-15 | 2024-06-20 | 天津巴莫科技有限责任公司 | Lithium-rich manganese-based positive electrode material, preparation method therefor, and use thereof |
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