CN108574098A - A kind of nanometer titanium dioxide-coated graphite lithium ion battery negative material and preparation method thereof - Google Patents
A kind of nanometer titanium dioxide-coated graphite lithium ion battery negative material and preparation method thereof Download PDFInfo
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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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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- 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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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
The invention discloses a kind of nanometer titanium dioxide-coated graphite lithium ion battery negative materials and preparation method thereof, and one layer of nano-TiO is uniformly coated in graphite surface by simple collosol and gel painting method2, nano-TiO2Coating thickness only 5 20nm, this 5 20nm thin layer uniformly coated make graphite surface have more effective electron transmission and in addition increase the interfacial surface area for storing lithium, improve cycle performance and high rate performance.
Description
Technical field：
The present invention relates to technical field of lithium ion, and in particular to a kind of nanometer titanium dioxide-coated graphite lithium ion electricity
Pond negative material and preparation method thereof.
Background technology：
In order to meet future portable electronics, the demand of EHV electric and hybrid vehicle, we have put into a large amount of energy
To develop advanced energy storage technology.Wherein lithium ion battery is due to its energy density height, and cycle performance is excellent, and self-discharge rate is small,
Memory effect is small and becomes more and more popular.Graphite is the most common negative material of lithium ion battery, and successfully realizes quotient
Industry.But its operating voltage is low, is easy to form Li dendrite, causes serious safety problem.Therefore, to graphite cathode material into
Row surface is modified, necessary with the chemical property for improving graphite.Nano-titanium dioxide (TiO2) have very high chemistry steady
It is qualitative and Li can be stored+Specific channel, and low cost, environmental sound.Its deintercalation current potential is avoided that lithium up to 1.5V
The formation of dendrite.Therefore, by one layer of TiO of Graphite Coating2Graphite electrochemistry performance can be improved.However, control reaction
Uniformly cladding is difficult completely for dynamics and realization, and extra titanium oligomer may condense together, and ultimately form TiO2
Particle, this is to TiO2Coating is also unfavorable.
Invention content：
The object of the present invention is to provide a kind of preparation sides of nanometer titanium dioxide-coated graphite lithium ion battery negative material
Method.
The present invention is achieved by the following technical programs：
A kind of preparation method of nanometer titanium dioxide-coated graphite lithium ion battery negative material, this method include following step
Suddenly：
(1) pretreatment of graphite：By 2-10g graphite dispersions in 200-800mL organic solvents, organic solvent is dioxy six
One or more of ring, cyclohexane, acetone, ethyl alcohol, propyl alcohol or acetone, ultrasonic 1-12h obtain the dilute suspension of graphite；
(2) TiO is prepared2Precursor solution：Titanium source, concentrated ammonia liquor are added in organic solvent, the organic solvent is with step
(1) organic solvent is consistent, and is sufficiently stirred to obtain TiO 2 precursor solution；The titanium source is tetraethyl titanate, metatitanic acid
One or more of orthocarbonate, butyl titanate, titanium source a concentration of 0.05-30wt%, ammonia concn 0.5-25wt%；
(3) precursor solution of step (2) preparation is slowly added drop-wise to the graphite that step (1) obtains by constant flow pump
In dilute suspension, at 20-80 DEG C being vigorously stirred 6-40h has been coated TiO2The graphite suspension of colloidal sol；Centrifugation filters
And gained graphite sample is collected, washing is dried to obtain dark gray powder；The drying is selected from spray drying, vacuum drying, freezing
It is any one of dry；
(4) powder sample obtained by step (3) is placed in tube furnace 450-700 DEG C of calcining 3-12h under an inert atmosphere, risen
1-5 DEG C of warm rate/min, obtains nano-TiO2Coated graphite ion cathode material lithium.
The inert atmosphere is selected from any one of nitrogen, argon gas and helium.
Beneficial effects of the present invention are as follows：
1), the present invention uniformly coats one layer of nano-TiO by simple sol-gel painting method in graphite surface2, receive
Rice TiO2Coating thickness only 5-20nm makes graphite surface have more effective electron transmission and in addition increase for storing lithium
Interfacial surface area improves cycle performance and high rate performance.This thin layer can be by providing short diffusion path to lithium ion.By
In graphite and nano-TiO2Maximized calmodulin binding domain CaM between crystal allow graphite surface be efficiently used for electron transmission and
In addition increase the interfacial surface area for storing lithium, this will promote electrochemical process and embodies excellent lithium storage characteristic.So
Nano-TiO prepared by the method for the present invention2Clad not only increases the electric conductivity of electrode, and avoids graphite and be in direct contact electricity
Xie Zhi, to reduce uncontrollable growth of SEI films.Illustrate nano-TiO2Coated graphite is as negative electrode of lithium ion battery material
The advantage of material：Excellent high rate capability and long cycle life.Nano-TiO will be coated2Graphite cathode material be applied to
The matched full battery of manganese-based anode material, considerably improves the cycle life of full battery.
2), the present invention avoids graphite from reuniting, is conducive to by ultrasound to Graphitic pretreatment using the cavitation of ultrasonic wave
Nano-TiO2Clad fully covers graphite surface.It is generally required with the prior art and adjusts the amount of water and acid simultaneously to control generation
The amount of titanium dioxide is different, and preparation method of the invention is more simple and convenient, is easy to control, and need to be by adjusting the content of alkali only
Controllable cladding TiO2Amount, can prepare with different-diameter, the even porous TiO of geometry and composition2, meet different
The demand of functional cells.
Description of the drawings：
Fig. 1 is the nano-TiO prepared by embodiment 12High magnification transmission electron microscope (TEM) figure of@C negative materials；
Fig. 2 is the TiO prepared by embodiment 12Scanning electron microscope (SEM) figure of@C negative materials；
Fig. 3 is the nano-TiO prepared by embodiment 12@C negative materials recycle 100 circles under the current density of 75mA/g
Cycle figure and efficiency chart.
Fig. 4 is the TiO prepared by embodiment 12@C are as cathode, LiNi0.5Mn1.5O4(LNMO) as the complete of anode assembling
Battery and blank graphite and the full battery of LNMO assemblings recycle the circulating effect comparison diagram of 50 circles under the current density of 30mA/g.
Specific implementation mode：
It is the further explanation to the present invention below, rather than limiting the invention.
Embodiment 1：A kind of nano-TiO2The preparation method of coated graphite lithium ion battery negative material
The pretreatment of graphite：By 3g graphite dispersions in 300mL dioxane, ultrasonic 2h obtains the dilute suspension of graphite.
TiO2It is prepared by precursor solution：By 2g butyl titanates, 100mL dioxane is added in 10mL concentrated ammonia liquors (28wt%)
In, butyl titanate concentration is about 2wt%, and ammonia concn 2.8wt% is sufficiently stirred to obtain TiO2Precursor solution.
Precursor solution is slowly added drop-wise in the dilute suspension of graphite by constant flow pump, is vigorously stirred at 70 DEG C
20h has been coated TiO2The graphite suspension of colloidal sol.Centrifugation filters and collects gained graphite sample, washing, and freezing is dry
It is dry, obtain dark gray powder.
Gained powder sample is placed in tube furnace calcines 3h for 700 DEG C under an inert atmosphere, and 5 DEG C/min of heating rate is obtained
Nano-TiO2Coated graphite ion cathode material lithium.Its high magnification transmission electron microscope (TEM) figure is as shown in Figure 1, display nano-TiO2's
A diameter of 5-20nm.Scanning electron microscope (SEM) figure is as shown in Fig. 2, be clearly illustrated on graphite cathode material complete and uniform
Nano-TiO2Coating.
Comparative example 1：A kind of nano-TiO2The preparation method of coated graphite lithium ion battery negative material
Include the following steps：
1,3g graphite dispersions are sufficiently mixed in the mixed solution of 6mL glacial acetic acid and 2mL water and 20mL absolute ethyl alcohols
To graphite mixed liquor；2, it is stirred at room temperature down, 2g butyl titanates and the mixed solution of 20mL absolute ethyl alcohols is slowly added drop-wise to
Step 1 obtains in the mixed liquor of graphite, has been coated TiO2The graphite suspension of colloidal sol is centrifuged or is filtered and collects gained stone
Black sample, washing, 120 DEG C of dryings obtain powder and are placed in tube furnace 700 DEG C under an inert atmosphere, calcine 34h under 0.01Mpa,
5 DEG C/min of heating rate, obtains nano-TiO2Coated graphite ion cathode material lithium.
Embodiment 2：A kind of nano-TiO2The preparation method of coated graphite lithium ion battery negative material
The pretreatment of graphite：By 10g graphite dispersions in 300mL cyclohexanes, ultrasonic 1h obtains the dilute suspension of graphite.
TiO2It is prepared by precursor solution：By 0.5g tetraethyl titanates, 10mL concentrated ammonia liquors are added in 100mL cyclohexanes, metatitanic acid
Four butyl esters a concentration of 0.5wt%, ammonia concn 2.8wt% are sufficiently stirred to obtain TiO2Precursor solution.
Precursor solution is slowly added in the dilute suspension of graphite by constant flow pump, is acutely stirred at 80 DEG C
20h is mixed, TiO has been coated2The graphite suspension of colloidal sol.
Graphite sample washs by centrifuging and collecting, dark gray powder is obtained after spray drying.By powder-like
Product are placed in tube furnace 450 DEG C of calcinings 4h, 1 DEG C/min of heating rate under an inert atmosphere and obtain nano-TiO2Coated graphite lithium
Ion negative material.
Embodiment 3：Electrochemical property test
The graphite sample (85wt%) that embodiment 1 or embodiment 2, comparative example 1 are obtained, polyvinylidene fluoride (PVDF)
(10wt%), carbon black (5wt%) and appropriate N-Methyl pyrrolidone (NMP) mixing are sized mixing, and are coated on copper foil and pole piece is made.By pole
Piece is placed in 110 DEG C of vacuum drying chambers and is dried overnight.It is made of lithium metal and CR2032 button cells is made to electrode.
Nano-TiO prepared by embodiment 12@C negative materials recycled under the current density of 75mA/g 50 circle cycle and
Efficiency chart (Fig. 3), as seen from the figure, capacity is almost without decaying after cycle, and coulombic efficiency is maintained at 98% or more, and the 50th circle is still
Specific discharge capacity with 345mAh/g, embodiment 2 have the effect of similar, and comparative example 1 is since clad is uneven, effect
Unobvious.Nano-TiO prepared by embodiment 12@C negative materials are as cathode, LiNi0.5Mn1.5O4(LNMO) as positive group
The full battery of dress recycles the cycle figures (Fig. 4) of 50 circles under the current density of 30mA/g, capacity and does not wrap as seen from the figure, after cycle
The full battery cycle performance of blank graphite assembling is covered compared to being obviously improved, and still there is 112mAh/g specific discharge capacities after 50 circles,
Though the effect for the full battery cycle performance non-ratio 1 that embodiment 2 assembles is good, also there are 90mAh/g specific discharge capacities after 50 circles, and
The full battery specific discharge capacity of uncoated blank graphite assembling only has 60mAh/g, and 1 effect of comparative example is similar with blank group, explanation
Only nano-TiO of the uniform fold in graphite surface2Clad is just avoided that electrolyte and graphite are in direct contact, and is avoiding manganese base just
Extremely dissolved manganese ion restores on the surface of graphite again, and active nano TiO2Li memory capacity is greatly increased, is promoted
Cycle performance.
Claims (2)
1. a kind of preparation method of nanometer titanium dioxide-coated graphite lithium ion battery negative material, which is characterized in that this method
Include the following steps：
(1) by 2-10g graphite dispersions in 200-800mL organic solvents, organic solvent is dioxane, cyclohexane, acetone, second
One or more of alcohol, propyl alcohol or acetone, ultrasonic 1-12h obtain the dilute suspension of graphite；
(2) titanium source, ammonium hydroxide are added in organic solvent, the organic solvent is consistent with step (1) organic solvent, is fully stirred
It mixes to obtain TiO 2 precursor solution；The titanium source be tetraethyl titanate, metatitanic acid orthocarbonate, one kind in butyl titanate or
It is several, titanium source a concentration of 0.05-30wt%, ammonia concn 0.5-25wt%；
(3) precursor solution prepared by step (2) the dilute of graphite that step (1) obtains slowly is added drop-wise to by constant flow pump to hang
In supernatant liquid, at 20-80 DEG C being vigorously stirred 6-40h has been coated TiO2The graphite suspension of colloidal sol；Centrifugation is filtered and is received
Collection gained graphite sample, washing are dried to obtain dark gray powder；The drying is selected from spray drying, vacuum drying, freeze-drying
Any one of；
(4) powder sample obtained by step (3) is placed in tube furnace 450-700 DEG C of calcining 3-12h under an inert atmosphere, heating speed
1-5 DEG C of rate/min, obtains nano-TiO2Coated graphite ion cathode material lithium.
2. the preparation method of nanometer titanium dioxide-coated graphite lithium ion battery negative material according to claim 1,
It is characterized in that, the inert atmosphere is selected from any one of nitrogen, argon gas and helium.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110311105A (en) * | 2019-06-20 | 2019-10-08 | 桑顿新能源科技(长沙)有限公司 | A kind of cathode pole piece slurry and preparation method, cathode pole piece, lithium ion battery |
| CN110323424A (en) * | 2019-05-29 | 2019-10-11 | 景德镇陶瓷大学 | The preparation method of titania modified molybdenum disulfide lithium ion battery negative material |
| CN111599995A (en) * | 2020-04-28 | 2020-08-28 | 惠州锂威新能源科技有限公司 | Cathode material, preparation method thereof and high-voltage lithium ion battery |
| CN111969185A (en) * | 2020-07-07 | 2020-11-20 | 湖南大学 | Coated TiO2Graphite double-ion battery composite positive electrode material and preparation method thereof |
| CN113206238A (en) * | 2021-05-12 | 2021-08-03 | 湖北亿纬动力有限公司 | NCM ternary cathode material, preparation method thereof and lithium ion battery |
| CN114242966A (en) * | 2021-11-12 | 2022-03-25 | 惠州锂威新能源科技有限公司 | Negative electrode composite material, preparation method thereof, negative electrode plate and secondary battery |
| CN114551836A (en) * | 2022-02-25 | 2022-05-27 | 蜂巢能源科技股份有限公司 | Negative electrode material, preparation method thereof, negative electrode sheet and battery |
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| CN110323424A (en) * | 2019-05-29 | 2019-10-11 | 景德镇陶瓷大学 | The preparation method of titania modified molybdenum disulfide lithium ion battery negative material |
| CN110311105A (en) * | 2019-06-20 | 2019-10-08 | 桑顿新能源科技(长沙)有限公司 | A kind of cathode pole piece slurry and preparation method, cathode pole piece, lithium ion battery |
| CN111599995A (en) * | 2020-04-28 | 2020-08-28 | 惠州锂威新能源科技有限公司 | Cathode material, preparation method thereof and high-voltage lithium ion battery |
| CN111969185A (en) * | 2020-07-07 | 2020-11-20 | 湖南大学 | Coated TiO2Graphite double-ion battery composite positive electrode material and preparation method thereof |
| CN111969185B (en) * | 2020-07-07 | 2022-04-01 | 湖南大学 | Coated TiO2Graphite double-ion battery composite positive electrode material and preparation method thereof |
| CN113206238A (en) * | 2021-05-12 | 2021-08-03 | 湖北亿纬动力有限公司 | NCM ternary cathode material, preparation method thereof and lithium ion battery |
| CN114242966A (en) * | 2021-11-12 | 2022-03-25 | 惠州锂威新能源科技有限公司 | Negative electrode composite material, preparation method thereof, negative electrode plate and secondary battery |
| CN114551836A (en) * | 2022-02-25 | 2022-05-27 | 蜂巢能源科技股份有限公司 | Negative electrode material, preparation method thereof, negative electrode sheet and battery |
| WO2023159863A1 (en) * | 2022-02-25 | 2023-08-31 | 蜂巢能源科技股份有限公司 | Negative electrode material and preparation method therefor, negative electrode plate and battery |
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