CN107452945A - A kind of preparation method of the lithium titanate anode material with nitrogen-doped carbon clad - Google Patents
A kind of preparation method of the lithium titanate anode material with nitrogen-doped carbon clad Download PDFInfo
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- CN107452945A CN107452945A CN201710575667.8A CN201710575667A CN107452945A CN 107452945 A CN107452945 A CN 107452945A CN 201710575667 A CN201710575667 A CN 201710575667A CN 107452945 A CN107452945 A CN 107452945A
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- H—ELECTRICITY
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Abstract
The invention belongs to technical field of lithium ion, more particularly to a kind of preparation method of the lithium titanate anode material with nitrogen-doped carbon clad, the present invention first uses lithium acetate etc. as lithium source, butyl titanate etc. is titanium source, cetyl trimethylammonium bromide is surfactant, prepares the nano barium titanate lithium material with high crystalline and chemical property；Recycle chemical vapor deposition method, it is carbon source and nitrogen source in the controllable nitrogen-doped carbon clad of flake lithium titanate material surface depositing homogeneous to use acetonitrile steam, so while lithium titanate material electric conductivity is improved, the preservation of lithium titanate sheet-like morphology is effectively facilitated, and then the circulation performance of lithium titanate battery is improved, and the problem of inhibit lithium titanate battery easy flatulence；In addition, the preparation method cost of the present invention is cheap, technique is simple, is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of lithium titanate with nitrogen-doped carbon clad is born
The preparation method of pole material.
Background technology
Because efficiency for charge-discharge is high, the features such as energy density is high, and environmental protection and cost are cheap, lithium ion battery is wide at present
It is general to be used on electronic product and power vehicle.The most wide negative material of currently commercially purposes surely belongs to graphite, but graphite is born
Pole because its charging/discharging voltage platform is relatively low, the defects of Li dendrite can be produced and pierce through barrier film and bring safety problem, grind at present
The person of the studying carefully positive new negative material of exploitation substitutes graphite cathode.
Wherein, spinel lithium titanate (Li4Ti5O12) lattice constant changes and is less than during Lithium-ion embeding with abjection
1%, it is referred to as " zero strain " material, is a kind of preferable embedding lithium electrode material.Simultaneously because have stable charge and discharge platform, well
Cycle performance, quickly charging property, higher heat endurance, cheap price and it is environment-friendly the features such as, become mesh
The study hotspot of preceding lithium ion battery negative material.
However, spinel lithium titanate has poor electron conduction and of a relatively high voltage platform, battery have impact on
Fast charging and discharging performance, particularly high rate capability performance, and flatulence easily occurs for common lithium titanate battery, influences
Battery performance and life-span, and then limit its application in electric automobile.
In order to improve lithium titanate electron conduction, by reducing particle size, can effectively reduce in charge and discharge process lithium from
Son and the diffusion length of electronics in the material, so as to reach quickening charge-discharge performance；Or design preparation has special appearance or one
Determine the lithium titanate of nanostructured, such as mesoporous microsphere, hollow microsphere, flower-like nanometer piece, can so increase the ratio surface of lithium titanate
Product, shorten lithium ion transport path, thus effectively improve the chemical property of lithium titanate；Can also by with carbon material (such as nothing
Setting carbon, CNT, graphene etc.) composite is prepared, promote the electricity of composite using the excellent electric conductivity of carbon material
Son and lithium ion transport, it is effectively improved the chemical property of lithium titanate anode material.But negative pole material made from above-mentioned improved method
Material often shows relatively low tap density and larger irreversible capacity, it is difficult to which the electrokinetic cell of high-energy-density is made.Cause
This, the design of high-tap density high-performance lithium titanate and the exploitation prepared to high energy density cells have highly important meaning
Justice.
The content of the invention
It is an object of the invention to：A kind of preparation side of the lithium titanate anode material with nitrogen-doped carbon clad is provided
Method, by simple and easy technique, prepare with nano-scale, the lithium titanate anode material that granule-morphology is uniform, purity is high
Material so that lithium titanate anode material has high specific capacity, good high rate performance and cycle performance, raising by a relatively large margin
The electric conductivity of lithium titanate anode material, and it is suitable for the production application of scale.
To achieve these goals, the present invention uses following technical scheme：
A kind of preparation method of the lithium titanate anode material with nitrogen-doped carbon clad, comprises the following steps：
Step 1: titanium source compound is added in cetyl trimethylammonium bromide solution, it is sufficiently stirred, then adds again
Add Li source compound solution, stir, obtain mixed solution；
Step 2: the mixed solution of step 1 is transferred in water heating kettle, carried out at 160~200 DEG C at hydro-thermal reaction
24~48h is managed, is then dried at 75~95 DEG C, and the powder after drying is placed in the tube furnace for being connected with inert gas
600~800 DEG C are heated to, 6~8h is incubated, obtains predecessor；
It is connected with Step 3: the predecessor that step 2 is obtained is placed in the tube furnace of inert gas and acetonitrile steam,
2~8h is incubated at 500~900 DEG C, that is, obtains the lithium titanate anode material with nitrogen-doped carbon clad.
Wherein, cetyl trimethylammonium bromide (CTAB) is not only successfully applied to as a kind of cationic surfactant
The synthesis of various crystalline materials (such as gold nanorods, gold nano grain), while also in energy field correlation nano-functional material
Important function has been played in preparation.
As the preferred scheme of the present invention, the content of titanium source compound described in step 1 is 5~150mmol.
As the preferred scheme of the present invention, the concentration of cetyl trimethylammonium bromide solution described in step 1 for 10~
100g/L。
As the preferred scheme of the present invention, the content of Li source compound described in step 1 is 1~100mmol.
As the preferred scheme of the present invention, titanium source compound described in step 1, the cetyl trimethylammonium bromide
Mol ratio with the Li source compound is 1:(0.05~0.5):(0.1~1).
As the preferred scheme of the present invention, titanium source compound described in step 1 is butyl titanate, tetraisopropyl titanate, two
Titanium oxide or titanium oxyoxalate.
As the preferred scheme of the present invention, Li source compound described in step 1 is lithium acetate, lithium sulfate, lithium oxalate, carbon
Sour lithium, lithium hydroxide, lithium chloride, lithium phosphate, lithium nitrate or lithium sulfide.
As the preferred scheme of the present invention, the flow velocity that inert gas described in step 3 and acetonitrile steam are passed through tube furnace is
150~250cm3/min。
As the preferred scheme of the present invention, the thickness of nitrogen-doped carbon clad described in step 3 is 2~40nm.
As the preferred scheme of the present invention, the inert gas is argon gas, nitrogen or helium.
Compared to prior art, the beneficial effects of the present invention are：The present invention first uses lithium acetate etc. as lithium source, metatitanic acid fourth
Ester etc. is titanium source, and cetyl trimethylammonium bromide is surfactant, prepares receiving with high crystalline and chemical property
Rice lithium titanate material；Chemical vapor deposition method is recycled, it is carbon source and nitrogen source in flake lithium titanate material to use acetonitrile steam
The controllable nitrogen-doped carbon clad of surface depositing homogeneous, so while lithium titanate material electric conductivity is improved, effectively facilitate
The preservation of lithium titanate sheet-like morphology, and then the circulation performance of lithium titanate battery is improved, and inhibit lithium titanate battery to hold
The problem of easy flatulence；In addition, the preparation method cost of the present invention is cheap, technique is simple, is suitable for large-scale industrial production.
Embodiment
To make technical scheme and advantage clearer, below in conjunction with specific embodiment, to the skill of the present invention
Art scheme is clearly and completely described, it is clear that and described embodiment is part of the embodiment of the present invention, rather than all
Embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art institute under the premise of creative work is not made
The every other embodiment obtained, belongs to the scope of protection of the invention.
Embodiment 1
A kind of preparation method of the lithium titanate anode material with nitrogen-doped carbon clad, it comprises the following steps：
Step 1), butyl titanate is added in cetyl trimethylammonium bromide solution, be sufficiently stirred, it is then slow again
Lithium acetate solution is added, stirs, obtains mixed solution, wherein, butyl titanate, cetyl trimethylammonium bromide and acetic acid
Mol ratio between lithium is 1：0.2：0.8；
Step 2), the mixed solution of step 1) is transferred in water heating kettle, carried out at 180 DEG C hydro-thermal reaction processing 24~
48h, then dried at 85 DEG C, and the powder after drying is placed in the tube furnace for be connected with argon gas and is heated to 700 DEG C, protected
Warm 7h, obtain predecessor nano-calcium carbonate lithium material；
Step 3), the nano-calcium carbonate lithium material that step 2 is obtained is evenly distributed in alumina crucible, is placed in leading to
In the tube furnace for having argon gas and acetonitrile steam, the flow velocity of argon gas and acetonitrile steam is 200cm3/ min, 4h is incubated at 700 DEG C,
Obtain the lithium titanate anode material with nitrogen-doped carbon clad.
Embodiment 2
A kind of preparation method of the lithium titanate anode material with nitrogen-doped carbon clad, it comprises the following steps：
Step 1), butyl titanate is added in cetyl trimethylammonium bromide solution, be sufficiently stirred, it is then slow again
Lithium hydroxide solution is added, stirs, obtains mixed solution, wherein, butyl titanate, cetyl trimethylammonium bromide and hydrogen
Mol ratio between lithia is 1：0.05：0.1；
Step 2), the mixed solution of step 1) is transferred in water heating kettle, carried out at 160 DEG C hydro-thermal reaction processing 24~
48h, then dried at 75 DEG C, and the powder after drying is placed in the tube furnace for be connected with argon gas and is heated to 600 DEG C, protected
Warm 8h, obtain predecessor nano-calcium carbonate lithium material；
Step 3), the nano-calcium carbonate lithium material that step 2 is obtained is evenly distributed in alumina crucible, is placed in leading to
In the tube furnace for having argon gas and acetonitrile steam, the flow velocity of argon gas and acetonitrile steam is 150cm3/ min, 8h is incubated at 500 DEG C,
Obtain the lithium titanate anode material with nitrogen-doped carbon clad.
Embodiment 3
A kind of preparation method of the lithium titanate anode material with nitrogen-doped carbon clad, it comprises the following steps：
Step 1), titanium dioxide is added in cetyl trimethylammonium bromide solution, be sufficiently stirred, it is then slow again
Lithium carbonate solution is added, stirs, obtains mixed solution, wherein, titanium dioxide, cetyl trimethylammonium bromide and carbonic acid
Mol ratio between lithium is 1：0.5：0.9；
Step 2), the mixed solution of step 1) is transferred in water heating kettle, carried out at 200 DEG C hydro-thermal reaction processing 24~
48h, then dried at 95 DEG C, and the powder after drying is placed in the tube furnace for be connected with argon gas and is heated to 800 DEG C, protected
Warm 6h, obtain predecessor nano-calcium carbonate lithium material；
Step 3), the nano-calcium carbonate lithium material that step 2 is obtained is evenly distributed in alumina crucible, is placed in leading to
In the tube furnace for having argon gas and acetonitrile steam, the flow velocity of argon gas and acetonitrile steam is 250cm3/ min, 2h is incubated at 900 DEG C,
Obtain the lithium titanate anode material with nitrogen-doped carbon clad.
Embodiment 4
A kind of preparation method of the lithium titanate anode material with nitrogen-doped carbon clad, it comprises the following steps：
Step 1), tetraisopropyl titanate is added in cetyl trimethylammonium bromide solution, be sufficiently stirred, Ran Houzai
Lithium oxalate solution is slowly added, is stirred, obtains mixed solution, wherein, tetraisopropyl titanate, cetyl trimethyl bromination
Mol ratio between ammonium and lithium oxalate is 1：0.1：0.5；
Step 2), the mixed solution of step 1) is transferred in water heating kettle, carried out at 180 DEG C hydro-thermal reaction processing 24~
48h, then dried at 85 DEG C, and the powder after drying is placed in the tube furnace for be connected with argon gas and is heated to 750 DEG C, protected
Warm 7h, obtain predecessor nano-calcium carbonate lithium material；
Step 3), the nano-calcium carbonate lithium material that step 2 is obtained is evenly distributed in alumina crucible, is placed in leading to
In the tube furnace for having argon gas and acetonitrile steam, the flow velocity of argon gas and acetonitrile steam is 200cm3/ min, 6h is incubated at 800 DEG C,
Obtain the lithium titanate anode material with nitrogen-doped carbon clad.
Embodiment 5
A kind of preparation method of the lithium titanate anode material with nitrogen-doped carbon clad, it comprises the following steps：
Step 1), titanium oxyoxalate is added in cetyl trimethylammonium bromide solution, be sufficiently stirred, it is then slow again
Lithium chloride solution is added, stirs, obtains mixed solution, wherein, titanium oxyoxalate, cetyl trimethylammonium bromide and chlorination
Mol ratio between lithium is 1：0.1：0.5；
Step 2), the mixed solution of step 1) is transferred in water heating kettle, carried out at 180 DEG C hydro-thermal reaction processing 24~
48h, then dried at 85 DEG C, and the powder after drying is placed in the tube furnace for be connected with argon gas and is heated to 650 DEG C, protected
Warm 7.5h, obtain predecessor nano-calcium carbonate lithium material；
Step 3), the nano-calcium carbonate lithium material that step 2 is obtained is evenly distributed in alumina crucible, is placed in leading to
In the tube furnace for having argon gas and acetonitrile steam, the flow velocity of argon gas and acetonitrile steam is 220cm3/ min, 5h is incubated at 700 DEG C,
Obtain the lithium titanate anode material with nitrogen-doped carbon clad.
Comparative example 1
Step 1), butyl titanate and lithium acetate mixed, be scattered in deionized water, stir, obtain mixed solution,
Wherein, the mol ratio between butyl titanate and lithium acetate is 1：0.8；
Step 2), the mixed solution of step 1) is transferred in water heating kettle, carried out at 180 DEG C hydro-thermal reaction processing 24~
48h, then dried at 85 DEG C, and the powder after drying is placed in the tube furnace for be connected with argon gas and is heated to 700 DEG C, protected
Warm 7h, obtain nano-calcium carbonate lithium material.
Comparative example 2
Step 1), butyl titanate is added in cetyl trimethylammonium bromide solution, be sufficiently stirred, it is then slow again
Lithium acetate solution is added, stirs, obtains mixed solution, wherein, butyl titanate, cetyl trimethylammonium bromide and acetic acid
Mol ratio between lithium is 1：0.2：0.8；
Step 2), the mixed solution of step 1) is transferred in water heating kettle, carried out at 180 DEG C hydro-thermal reaction processing 24~
48h, then dried at 85 DEG C, and the powder after drying is placed in the tube furnace for be connected with argon gas and is heated to 700 DEG C, protected
Warm 7h, obtain predecessor nano-calcium carbonate lithium material；
Step 3), the nano-calcium carbonate lithium material that step 2 is obtained is evenly distributed in alumina crucible, is placed in leading to
Have in the tube furnace of argon gas, the flow velocity of argon gas is 200cm3/ min, is incubated 4h at 700 DEG C, that is, obtains having carbon coating layer
Lithium titanate anode material.
Comparative example 3
(1) 50g titanium dioxide and 19.42g lithium carbonates are taken respectively, while add 1.38g glucose and 55.54g ball millings help
Agent absolute ethyl alcohol, ball milling mixing 15h is carried out, is then dried；
(2) high-temperature process：Under inert gas shielding, the powder of drying in step (2) is heated to 900 with 5 DEG C/min
DEG C, continue 4 hours, after cooling down to room temperature, pulverize and sieve, that is, obtain carbon coating lithium titanate anode material.
To examine the performance of the lithium titanate anode material of the inventive method preparation, respectively to using embodiment 1~5 and contrast
Half-cell made of the negative material of example 1~3 carries out electrochemical property test.
Tested with half-cell method of testing, specifically, using the negative material of above example and comparative example：Acetylene
It is black：PVDF=93：3：4 (weight ratios), add appropriate NMP to be tuned into slurry, are coated on copper foil, are made through the drying 8 hours of 110 DEG C of vacuum
Into negative plate；Using metal lithium sheet as to electrode, electrolyte is 1mol/L LiPF6/ EC+DEC+DMC (wherein volume ratio EC：DEC：
DMC=1：1：1), microporous polypropylene membrane is barrier film, is assembled into battery.
Electrochemical property test the results are shown in Table 1.
The electrochemical property test result of the negative material of the embodiment of table 1 and comparative example
From the test result of table 1, surfactant is used compared to useless, also without the comparative example for carrying out carbon coating
1, the tap density for the lithium titanate anode material that preparation method of the present invention obtains, first electrical conductivity, discharging efficiency, circulation volume guarantor
Specific capacity under holdup and identical multiplying power is significantly superior different；And compared to not using acetonitrile steam progress nitrogen-doped carbon cladding
Comparative example 2 and the comparative example 3 of carbon coating is carried out using conventional method, the lithium titanate anode that preparation method of the present invention obtains
Electrical conductivity, the circulation performance of material are considerably higher, because the present invention can as carbon source and nitrogen source by the use of acetonitrile steam
Effectively facilitate the preservation of lithium titanate sheet-like morphology, the nitrogen-doped carbon clad of formation uniformly, be densely coated on lithium titanate material
Surface, effectively stable lithium titanate material structure, and also the introducing of nitrogen-atoms can destroy C-C keys in carbon coating layer, form it into carbon
Layer defects, be so advantageous to the diffusion of lithium ion to a certain extent, so as to effectively improve the electrical conductivity of lithium titanate material, multiplying power
Cycle performance.
The announcement and teaching of book according to the above description, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and changed.Therefore, the invention is not limited in above-mentioned embodiment, every those skilled in the art exist
Made any conspicuously improved, replacement or modification belong to protection scope of the present invention on the basis of the present invention.This
Outside, although having used some specific terms in this specification, these terms merely for convenience of description, not to the present invention
Form any restrictions.
Claims (10)
1. a kind of preparation method of the lithium titanate anode material with nitrogen-doped carbon clad, it is characterised in that including following step
Suddenly：
Step 1: titanium source compound is added in cetyl trimethylammonium bromide solution, it is sufficiently stirred, then adds lithium again
Source compound solution, stirs, and obtains mixed solution；
Step 2: the mixed solution of step 1 is transferred in water heating kettle, hydro-thermal reaction processing 24 is carried out at 160~200 DEG C
~48h, then dried at 75~95 DEG C, and the powder after drying is placed in the tube furnace for be connected with inert gas and heated
To 600~800 DEG C, 6~8h is incubated, obtains predecessor；
It is connected with Step 3: the predecessor that step 2 is obtained is placed in the tube furnace of inert gas and acetonitrile steam, 500~
2~8h is incubated at 900 DEG C, that is, obtains the lithium titanate anode material with nitrogen-doped carbon clad.
2. the preparation method of the lithium titanate anode material according to claim 1 with nitrogen-doped carbon clad, its feature
It is：The content of titanium source compound described in step 1 is 5~150mmol.
3. the preparation method of the lithium titanate anode material according to claim 1 with nitrogen-doped carbon clad, its feature
It is：The concentration of cetyl trimethylammonium bromide solution described in step 1 is 10~100g/L.
4. the preparation method of the lithium titanate anode material according to claim 1 with nitrogen-doped carbon clad, its feature
It is：The content of Li source compound described in step 1 is 1~100mmol.
5. the preparation method of the lithium titanate anode material according to claim 1 with nitrogen-doped carbon clad, its feature
It is：The mol ratio of titanium source compound described in step 1, the cetyl trimethylammonium bromide and the Li source compound
For 1:(0.05~0.5):(0.1~1).
6. the preparation method of the lithium titanate anode material according to claim 1 with nitrogen-doped carbon clad, its feature
It is：Titanium source compound described in step 1 is butyl titanate, tetraisopropyl titanate, titanium dioxide or titanium oxyoxalate.
7. the preparation method of the lithium titanate anode material according to claim 1 with nitrogen-doped carbon clad, its feature
It is：Li source compound described in step 1 is lithium acetate, lithium sulfate, lithium oxalate, lithium carbonate, lithium hydroxide, lithium chloride, phosphoric acid
Lithium, lithium nitrate or lithium sulfide.
8. the preparation method of the lithium titanate anode material according to claim 1 with nitrogen-doped carbon clad, its feature
It is：The flow velocity that inert gas described in step 3 and acetonitrile steam are passed through tube furnace is 150~250cm3/min。
9. the preparation method of the lithium titanate anode material according to claim 1 with nitrogen-doped carbon clad, its feature
It is：The thickness of nitrogen-doped carbon clad described in step 3 is 2~40nm.
10. the preparation method of the lithium titanate anode material according to claim 1 with nitrogen-doped carbon clad, its feature
It is：The inert gas is argon gas, nitrogen or helium.
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| CN108417824B (en) * | 2018-03-06 | 2020-10-09 | 辽宁大学 | Preparation method of high-performance lithium battery cathode material carbon-coated lithium titanate |
| CN108520953A (en) * | 2018-04-17 | 2018-09-11 | 吉林大学 | A kind of carbon coating lithium titanate negative material and preparation method thereof |
| WO2023241152A1 (en) * | 2022-06-16 | 2023-12-21 | 天津大学 | Preparation method for hollow nitrogen-doped carbon-coated titanium dioxide photocatalyst |
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