CN108417824A - A kind of preparation method of high-performance lithium battery negative material carbon cladding lithium titanate - Google Patents
A kind of preparation method of high-performance lithium battery negative material carbon cladding lithium titanate Download PDFInfo
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- CN108417824A CN108417824A CN201810182435.0A CN201810182435A CN108417824A CN 108417824 A CN108417824 A CN 108417824A CN 201810182435 A CN201810182435 A CN 201810182435A CN 108417824 A CN108417824 A CN 108417824A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
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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
The present invention discloses a kind of preparation method of high-performance lithium battery negative material carbon cladding lithium titanate.Specially：At room temperature, CTAB is dissolved in isopropanol, magnetic agitation is uniformly mixed；Then butyl titanate is added dropwise, lithium hydroxide aqueous solution is added dropwise again in gained mixed solution, after stirring, mixture is transferred in stainless steel autoclave, 36h is kept at 180 DEG C, obtains white precipitate；Centrifuge washing, it is dry in 85 DEG C of baking oven, by gained presoma in tube furnace, 6h is calcined at 700~750 DEG C, cooling, grinding obtains target product.The present invention innovatively selects CTAB as structure directing agent, the narrow lithium titanate Li of oriented growth grain size4Ti5O12Nano material forms the special construction of carbon coating lithium titanate, and the chemical properties such as high rate performance, cycle performance for significantly increasing the lithium ion of lithium titanate and the efficiency of transmission of electronics, and then leading to material itself are better.
Description
Technical field
The present invention relates to technical field of lithium ion, more particularly to a kind of high-performance lithium battery negative material carbon coats titanium
The preparation method of sour lithium.
Background technology
Human society is fast-developing with the progress of science and technology, but the problems such as also result in environmental pollution, resource exhaustion.
Since the 21th century, the mankind gradually recognize that exploitation is novel while enjoying high-quality life caused by scientific development
The importance of clean energy resource.In numerous new cleaning fuels, lithium ion battery is due to small, light weight, energy
Density is big, good cycling stability, self discharge are small, memory-less effect, the prominent advantage such as safe and reliable, pollution-free, has attracted
Researcher widely pays close attention to.
An important factor for lithium ion battery negative material is as the energy content of battery, high rate performance and cycle life is improved manages institute
It should be favored by researcher.In lithium ion battery, the negative material of exploitation includes mainly carbon negative pole material, germanium base cathode
Material, silicon based anode material, titanium-based negative material (Li4Ti5O12) etc., and titanium-based negative material (Li4Ti5O12) intrinsic with it
Characteristic causes the extensive concern of researcher, spinel lithium titanate (Li4Ti5O12) 1.55V (vs.Li/Li+) have it is flat and
Spacious charge and discharge platform, while during charge and discharge, material itself only has 0.2% volume change, for one kind, " zero answers
Become " negative material, therefore have excellent stability.But spinel lithium titanate (Li4Ti5O12) there are poorly conductive, lithium ions
With electronics transmission efficiency is low two serious disadvantages, the shortcomings that researcher surrounds these two aspects, is modified it excellent
Change.At present frequently with spinel lithium titanate negative material modified optimization method, including nanosizing shorten Li+With electronics in material
Transmission range inside material；It prepares composite system and constructs conductive net, improve Li+With the transport capability of electronics；Doping changes
Property optimization, reduce electrode polarization of the material under high magnification, improve electron transport ability of material etc..
With the progress of the development and civilization of social economy, people increase severely to the demand of the energy with day, to novel green
The exploitation of the energy is very urgent.Lithium ion battery causes the extensive research of scientific research personnel as a kind of green high-efficient energy storage material
Interest.And lithium ion battery negative material is the key that ensure that li-ion electrode has one of high-energy-density and cyclical stability.
Some novel titanium-based negative material (such as Li4Ti5O12) extensive concern of people and great research interest are caused, also have very much uncommon
It hopes and realizes commercialization, be applied to next-generation high performance lithium ion battery, to push the continuous development of lithium ion battery, to alleviate
Energy crisis pushes development of human civilization to contribute.
Invention content
In order to solve the problems, such as that transmission efficiency is low for lithium ion and electronics in lithium ionic cell cathode material lithium titanate, this hair
Bright is designed to provide a kind of preparation method of high-performance lithium battery negative material carbon cladding lithium titanate, to further increase it
Chemical property.
The technical solution adopted by the present invention is：A kind of preparation side of high-performance lithium battery negative material carbon cladding lithium titanate
Method includes the following steps：
1) at room temperature, cetyltrimethylammonium bromide (CTAB) is dissolved in isopropanol, magnetic agitation, mixing is equal
It is even, butyl titanate is added, obtains mixed solution；
2) in the mixed solution obtained by step 1), lithium hydroxide aqueous solution is added, after stirring 4~5h, reaction solution is turned
It moves on in stainless steel autoclave, 36~45h of reaction at 175~185 DEG C, gained white precipitate, after centrifuge washing, in 85 DEG C of baking
It is dry in case, obtain presoma；
3) presoma obtained by step 2) is placed in tube furnace, in nitrogen atmosphere, calcine 6 at 600~750 DEG C~
7h, cooled to room temperature, grinding obtain target product.
Above-mentioned preparation method, lithium hydroxide and butyl titanate are 4.5 according to lithium titanium molar ratio:5 carry out dispensing.
The feed postition of above-mentioned preparation method, butyl titanate and lithium hydroxide aqueous solution is to be added dropwise.
Above-mentioned preparation method, calcination temperature are 700~750 DEG C.
The beneficial effects of the invention are as follows：
The preparation method of high-performance lithium battery negative material carbon cladding lithium titanate provided by the invention, using isopropanol-water
The hot method of double solvents, with butyl titanate and LiOHH2O is raw material, using isopropanol, water as solvent, in 175~185 DEG C of temperature
Under, presoma is made in 36~45h of reaction；By presoma in nitrogen atmosphere, high temperature sintering obtains target product Li4Ti5O12/C.It is logical
Cross the nanometer Li that this method is prepared4Ti5O12/ C-material not only solves metatitanic acid under the premise of keeping LTO good characteristics
The lithium ion and electronics of lithium the problem of transmission efficiency is low, and particular, it is important that its microstructure further increases material
The specific surface area of material, and then improve the chemical property of material.And use the extremely simple hot method of isopropanol-water double solvents
One-step synthesis is particularly conducive to realize the commercialization of LTO electrode materials, pushes the process of lithium ion battery negative material development.
The present invention innovatively selects CTAB as structure directing agent, the narrow metatitanic acid of oriented growth grain size in preparation process
Lithium Li4Ti5O12Nano material, prepared nano material have larger specific surface area, have when with electrolyte contacts more
Active contact site.CTAB provides suitable carbon source for the synthesis of the composite material simultaneously, the titanium in inert atmosphere calcination process
Sour lithium surface has micro Carbon deposition and gets off, and forms the special construction of carbon coating lithium titanate in this way, significantly increases lithium titanate
The efficiency of transmission of lithium ion and electronics, and then the chemical properties such as high rate performance, cycle performance for leading to material itself are better.
Description of the drawings
Fig. 1 is Li obtained by 700~750 DEG C of temperature calcinations4Ti5O12The XRD diagram of/C.
Fig. 2 is Li obtained by 600~650 DEG C of temperature calcinations4Ti5O12The XRD diagram of/C.
Fig. 3 is Li obtained by 700~750 DEG C of temperature calcinations4Ti5O12The SEM image of/C；
Wherein, a：1μm；b：500nm.
Specific implementation mode
The guarantor that the present invention is further explained, but is not intended to restrict the invention with reference to specific embodiment
Protect range.
The preparation method of high-performance lithium battery negative material carbon cladding lithium titanate provided by the invention, includes the following steps：
1) at room temperature, cetyltrimethylammonium bromide (CTAB) is dissolved in isopropanol, magnetic agitation 4h, mixing is equal
It is even；Then butyl titanate is added dropwise, obtains mixed solution；
2) in deionized water by lithium hydroxide dissolving, after magnetic agitation is completely dissolved, lithium hydroxide aqueous solution is obtained.By hydrogen
Lithia aqueous solution is added dropwise in the mixed solution obtained by step 1), and after stirring 5h, mixture is transferred to stainless steel height
It presses in kettle, and reacts 36~45h at 175~185 DEG C, white precipitate is obtained after hydro-thermal process；Centrifuge washing 5 times, and 85
DEG C baking oven in it is dry, obtain presoma；
3) presoma obtained by step 2) is put into tube furnace, respectively to forge at a temperature of 700~750 DEG C, 600~650 DEG C
It burns 6 hours, cooled to room temperature, grinding respectively obtains target product Li4Ti5O12/C。
Wherein, in order to keep material electrochemical performance obtained better, the dosage of CTAB is suitable in step 1), i.e., often
10mmol butyl titanates and 9mmol lithium hydroxides is added in 0.2g CTAB.The molar ratio of lithium and titanium is 4.5:5, lithium needed
For amount, which is because, during step 3) high-temperature calcination, lithium source has loss, if lithium is not excessive, can generate impurity
TiO2.The purpose that step 3) carries out high-temperature calcination in nitrogen atmosphere is, converts presoma under the high temperature conditions in sharp crystalline substance
Stone lithium titanate Li4Ti5O12Negative material, while CTAB can be converted into carbon source in inert atmosphere.
In order to really enable raw material lithium hydroxide and butyl titanate fully react, as the improvement of technical solution, by hydrogen
Lithia is added in a manner of being added dropwise.
Wherein, by LiOHH in step 2)2O is placed in the stirring in deionized water, preferably magnetic agitation, is stirred with control
Speed is mixed, uniformity coefficient is improved.
The temperature calcined in step 3) is preferably 700~750 DEG C.
Embodiment 1
High-performance lithium battery negative material carbon coats the preparation method of lithium titanate, includes the following steps：
1) at room temperature, 0.2g cetyltrimethylammonium bromide (CTAB) is dissolved in 30mL isopropanols, magnetic agitation
4h is uniformly mixed；Then 10mmol butyl titanates are added dropwise, obtain mixed solution；
2) 9mmol lithium hydroxides are dissolved in 15mL deionized waters, after magnetic agitation is completely dissolved, obtain lithium hydroxide water
Solution.Lithium hydroxide aqueous solution is added dropwise in the mixed solution obtained by step 1), 5h is stirred, then shifts mixture
Into 100mL stainless steel autoclaves, and 36h is reacted at 175~185 DEG C, white precipitate is obtained after hydro-thermal process；Centrifuge washing 5
It is secondary and dry in 85 DEG C of baking oven, presoma is made；
3) presoma obtained by step 2) is put into tube furnace, 600~650 DEG C of temperature lower calcinations 6 hours naturally cool to
Target product Li is made in room temperature, grinding4Ti5O12/C。
Embodiment 2
High-performance lithium battery negative material carbon coats the preparation method of lithium titanate, includes the following steps：
1) at room temperature, 0.2g cetyltrimethylammonium bromide (CTAB) is dissolved in 30mL isopropanols, magnetic agitation
4h is uniformly mixed；Then 10mmol butyl titanates are added dropwise, obtain mixed solution；
2) 9mmol lithium hydroxides are dissolved in 15mL deionized waters, after magnetic agitation is completely dissolved, obtain lithium hydroxide water
Solution.Lithium hydroxide aqueous solution is added dropwise in the mixed solution obtained by step 1), 5h is stirred, then shifts mixture
Into 100mL stainless steel autoclaves, and 36h is reacted at 175~185 DEG C, white precipitate is obtained after hydro-thermal process；Centrifuge washing 5
It is secondary and dry in 85 DEG C of baking oven, presoma is made；
3) presoma obtained by step 2) is put into tube furnace, 700~750 DEG C of temperature lower calcinations 6 hours naturally cool to
Target product Li is made in room temperature, grinding4Ti5O12/C。
The Li that embodiment 1 and embodiment 2 are obtained4Ti5O12/ C carries out XRD and SEM detections, as a result as shown in Figure 1, Figure 2 and Fig. 3
It is shown.
As shown in Figure 1, the target product Li that embodiment 1 obtains4Ti5O12/ C purity is high, and XRD diffraction maximums are sharp, with metatitanic acid
Lithium standard card (JCPDS card numbers：It 49-0207) compares, has no the appearance of other miscellaneous peaks.
As shown in Figure 2, the target product Li that embodiment 2 obtains4Ti5O12/ C, the spectrogram show some TiO2Impurity peaks,
It is sharp that XRD diffraction maximums are also not so good as Fig. 1 XRD diffraction maximums.
As seen from Figure 3, the target product Li that embodiment 1 obtains4Ti5O12/ C, grain size is relatively narrow, and pattern is more regular.
Embodiment 3
For embodiment 1, the bought LTO materials of 2 resulting materials of embodiment and common market, using it as battery cathode
Material, lithium piece are used as to electrode, are assembled into button cell, carry out electrochemical property test to it, the results are shown in Table 1.
The different negative material chemical properties of table 1 compare (charge-discharge magnification 1C)
By table 1 as it can be seen that compared to common LTO negative materials, the high-performance lithium battery cathode of method of the invention synthesis
Material of lithium titanate Li4Ti5O12The chemical property of/C is improved significantly, and can be seen that 700~750 DEG C of temperature lower calcination institutes
Obtained material, chemical property is significantly larger than with obtained by calcining under the conditions of 600~650 DEG C of good chemical property
Material；Innovatively select CTAB as the structure directing agent of the material, the narrow titanium of oriented growth grain size in this preparation process
Sour lithium Li4Ti5O12Nano material, the nano material have larger specific surface area, there is more activity when with electrolyte contacts
Site is contacted, while CTAB provides suitable carbon source for the synthesis of the composite material, the lithium titanate in inert atmosphere calcination process
Surface has micro Carbon deposition and gets off, and forms the special construction of carbon coating lithium titanate in this way, significantly increase the lithium of lithium titanate from
The efficiency of transmission of son and electronics, and then the chemical properties such as high rate performance, cycle performance for leading to material itself are better.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of preparation method of high-performance lithium battery negative material carbon cladding lithium titanate, which is characterized in that include the following steps：
1) at room temperature, cetyltrimethylammonium bromide is dissolved in isopropanol, magnetic agitation, is uniformly mixed, metatitanic acid is added
Four butyl esters, obtain mixed solution；
2) in the mixed solution obtained by step 1), lithium hydroxide aqueous solution is added, after stirring 4~5h, reaction solution is transferred to
In stainless steel autoclave, 36~45h, gained white precipitate, after centrifuge washing, in 85 DEG C of baking oven are reacted at 175~185 DEG C
It is dry, obtain presoma；
3) presoma obtained by step 2) is placed in tube furnace, in nitrogen atmosphere, 6~7h is calcined at 600~750 DEG C, from
It is so cooled to room temperature, grinds, obtain target product.
2. preparation method described in accordance with the claim 1, which is characterized in that lithium hydroxide and butyl titanate are according to lithium titanium mole
Than being 4.5:5 carry out dispensing.
3. preparation method described in accordance with the claim 1, which is characterized in that the addition of butyl titanate and lithium hydroxide aqueous solution
Mode is to be added dropwise.
4. preparation method described in accordance with the claim 1, which is characterized in that calcination temperature is 700~750 DEG C.
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Cited By (2)
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| CN111653748A (en) * | 2020-06-04 | 2020-09-11 | 松山湖材料实验室 | Ge-GeO2-TiO2Preparation method of-C nanocomposite material, product and application thereof |
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