CN105789583B - A kind of lithium ion battery negative material Li4Ti5O12/TiO2/ Ag and preparation method thereof - Google Patents
A kind of lithium ion battery negative material Li4Ti5O12/TiO2/ Ag and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of lithium ion battery negative material Li4Ti5O12/TiO2/ Ag and preparation method thereof uses the straightforward procedure that hydrolysis is assisted and further calcined to prepare Li4Ti5O12/TiO2Material；Then, and AgNO is used3Thermal decomposition is subject to ultrasonic wave added and target product Li is made in a manner of deposited metal Ag4Ti5O12/TiO2/ Ag composite materials.Preparation method provided by the invention is easy, easy to operate, is nano particle structure by the lithium ion battery negative material that this method is prepared, increases the specific surface area of material；Keeping spinel-type Li simultaneously4Ti5O12Under the premise of good characteristic, TiO has been had both2And the advantage of metal Ag, further improve its chemical property as lithium ion battery negative material.
Description
Technical field
The present invention relates to technical field of lithium ion, specifically provide a kind of lithium ion battery negative material
Li4Ti5O12/TiO2/ Ag and preparation method thereof.
Background technology
At present, negative material used in high multiplying power lithium ion battery is mainly graphite-like carbon material, such material is maximum to ask
Topic is that its surface easily forms Li dendrite during large current charge, to seriously affect the performance of material capacity and thus draw
Send out safety issue.Spinel-type Li4Ti5O12(LTO) it is a kind of " zero strain " material, this special performance makes it in lithium
Ion insertion/it is embedding go out during have good invertibity；Moreover, Li4Ti5O12There is stable, higher operating voltage (about
1.55V, vs Li+/ Li), this can be to avoid the formation of Li dendrite and the generation of SEI films, to improve battery security.
Just because of the two features, Li4Ti5O12As most promising lithium ion battery negative material；However, its low electronics
Electric conductivity and weak lithium ion diffusivity affect lithium ion battery high rate capability, and then limit it and answer on a large scale
With.
So far, researchers take many measures to improve LTO electronics and ionic conductivity, including synthesis is received
Rice material, bulk phase-doped and high conductivity material cladding etc..
In recent years, a few studies person was dedicated to developing Ag load LTO materials, to improve the electron conduction of LTO, in turn
Improve its high rate capability and cycle performance, and achieves good achievement.Meanwhile Rutile-TiO2It is embedding in lithium ion
Enter-deintercalation process medium-rate is fast, there are higher capacity and good cyclical stability.It is reported that for lithium ion battery
Cathode, about Li4Ti5O12/TiO2The research of/Ag composite materials is seldom reported.
Invention content
The purpose of the present invention is to provide a kind of lithium ion battery negative material Li4Ti5O12/TiO2/ Ag and its preparation side
Method, with provide it is a kind of be simple and efficient method prepare with excellent properties lithium ion battery negative material.
Technical solution provided by the invention, specifically, a kind of lithium ion battery negative material Li4Ti5O12/TiO2/ Ag's
Preparation method includes the following steps：
1) under room temperature, butyl titanate is placed in absolute ethyl alcohol, stirs and is sufficiently mixed 1h, obtain solution A；Then
By CH3COOLi·2H2O is dissolved in a small amount of deionized water, fully after dissolving, is added in above-mentioned solution A, under drying condition, reaction
10-12h obtains milky reaction solution；
2) milky reaction solution is placed under 90 DEG C of equal tepidariums and reacts 1h；Then, it is dried in vacuo 6-8h in 70-80 DEG C,
Obtain intermediate product presoma；
3) intermediate product presoma is placed in air atmosphere, 590-800 DEG C of calcining 6-7h cools to room temperature with the furnace, grind
Mill, obtains intermediate product Li4Ti5O12/TiO2。
4) appropriate AgNO at room temperature, is taken3With made Li4Ti5O12/TiO2In deionized water, after ultrasonic disperse 2h, 70-
80 DEG C of vacuum drying 6-8h, obtain target product precursor powder；It then grinds, 500 DEG C of calcinings in Muffle furnace under air atmosphere
2h obtains target product Li4Ti5O12/TiO2/Ag。
It is preferred that CH in step 1)3COOLi·2H2O and butyl titanate are according to molar ratio Li：Ti=4:5~5.5 carry out
Dispensing.
Further preferably, CH in step 1)3COOLi·2H2The feed postition of O solution is to be added dropwise.
Further preferably, stirring is magnetic agitation in step 1).
Further preferably, the temperature calcined in step 3) is 690-700 DEG C.
Further preferably, in step 4) Ag to Li4Ti5O12/TiO2Mass percent be 3-8wt%, specially 3wt%,
5wt% and 8wt%, to preferably go out the dosage of best Ag.
The present invention also provides a kind of lithium ion battery negative material Li4Ti5O12/TiO2/ Ag, the negative material is by upper
Any one method is stated to be prepared.
Lithium ion battery negative material Li provided by the invention4Ti5O12/TiO2/ Ag and preparation method thereof uses hydrolysis
Auxiliary and the straightforward procedure further calcined prepare Li4Ti5O12/TiO2Material；Then, and AgNO is used3Thermal decomposition is with heavy
The mode of product metal Ag, and target product Li is made in the mode for being subject to ultrasonic wave added4Ti5O12/TiO2/ Ag composite materials.This hair
The preparation method of bright offer is easy, easy to operate, is nano-particle by the lithium ion battery negative material that this method is prepared
Structure increases the specific surface area of material；Keeping spinel-type Li simultaneously4Ti5O12Under the premise of good characteristic, have both
TiO2And the advantage of metal Ag, further improve its chemical property as lithium ion battery negative material when.The party
Lithium ion battery negative material Li prepared by method4Ti5O12/TiO2/ Ag is advantageously implemented Li4Ti5O12The commercialization of electrode material,
To promote its large-scale practical application.
Description of the drawings
Fig. 1 is that different temperatures calcines gained intermediate product Li4Ti5O12/TiO2XRD diagram；Wherein, a, 590-600 DEG C；b、
690-700℃；c、790-800℃.
Fig. 2 is 690-700 DEG C of calcining gained intermediate product Li4Ti5O12/TiO2It is further processed the battery cathode material of gained
Expect Li4Ti5O12-TiO2The XRD diagram of/Ag；Wherein, Ag is to Li4Ti5O12/TiO2Mass percent be respectively a, 3wt%；b、
5wt%；C, 8wt%.
Specific implementation mode
The present invention is further expalined with reference to specific embodiment, but be not intended to restrict the invention
Protection domain.
In order to further improve preparation process present in the application range and preparation method of lithium ion battery negative material
The problems such as complicated, not easy to control, present embodiment provides a kind of lithium ion battery negative material Li4Ti5O12/TiO2/ Ag's
Simple preparation method includes the following steps：
1) under room temperature, butyl titanate is placed in absolute ethyl alcohol, stir and is sufficiently mixed 1h；Then will
CH3COOLi·2H2O is dissolved in a small amount of deionized water, fully after dissolving, is added in above-mentioned solution, under drying condition, reacts 10-
12h obtains milky reaction solution；
2) milky white solution is placed under 90 DEG C of equal tepidariums and reacts 1h；Then, it is dried in vacuo 6- in 70-80 DEG C
8h obtains intermediate product presoma；
3) the product presoma is placed in air atmosphere, 590-800 DEG C of calcining 6-7h cools to room temperature with the furnace, grind
Mill, obtains intermediate product Li4Ti5O12/TiO2。
4) appropriate AgNO at room temperature, is taken3With made Li4Ti5O12/TiO2In deionized water, after ultrasonic disperse 2h, 70-
80 DEG C of vacuum drying 6-8h, obtain target product precursor powder；It then grinds, 500 DEG C of calcinings in Muffle furnace under air atmosphere
2h obtains Li4Ti5O12/TiO2/ Ag target products.
Wherein, it in order to ensure obtained negative material can show good chemical property, is selected in step 1)
Two kinds of raw material Li sources and the sources Ti, the two be necessary for liquid, so as to better haptoreaction, thus need using absolute ethyl alcohol it is molten
Butyl titanate is solved, and magnetic agitation 1h makes it be sufficiently mixed；CH is added dropwise simultaneously3COOLi·2H2O aqueous solutions, otherwise
Tetrabutyl titanate hydrolysis in ethyl alcohol is too fast, keeps solution uneven；The CH of usual 0.530-0.550g3COOLi·2H2O needs big
The deionized water dissolving of about 10-12ml.Consider, it is 17-25ml to test absolute ethyl alcohol used.
Step 2) is fully dry by milky white solution, and grinding obtains intermediate product presoma.
The purpose calcined in air atmosphere in step 3) is to convert presoma to centre under the high temperature conditions
Product Li4Ti5O12/TiO2。
It is to make Li that ultrasonic disperse is selected in step 4)4Ti5O12/TiO2With AgNO3It is sufficiently mixed；500 DEG C of calcinings are selected, are
Because of AgNO3Heat decomposition temperature be about 440 DEG C, obtain Ag to react decomposition, and then form target product.
In order to ensure obtained negative material is the preferable nano-particle distribution of dispersibility, to increase the ratio table of material
Area improves the chemical property of material, it is preferable that two kinds of raw material CH3COOLi·2H2O and butyl titanate are according to molar ratio Li/
Ti=4:5~5.5 carry out dispensing, to ensure the intermediate product to be formed for Li4Ti5O12/TiO2。
In order to ensure two kinds of raw material CH3COOLi·2H2O and butyl titanate can fully be reacted, butyl titanate
Hydrolysis rate it is also unsuitable too fast, as the improvement of technical solution, CH3COOLi·2H2The feed postition of O aqueous solutions is to add dropwise
Enter.
Wherein, the stirring involved in step 1), preferably magnetic agitation carry so as to preferably control mixing speed
High uniformity coefficient, and it is easy to operate.
The temperature calcined in step 3) is preferably 690-700 DEG C.
Ag is to Li in step 4)4Ti5O12/TiO2Mass percent be 3-8wt%, preferably 5wt%.
The preparation method further illustrated the present invention with reference to specific embodiment.
A kind of 1 lithium ion battery negative material Li of embodiment4Ti5O12/TiO2The intermediate product Li of/Ag4Ti5O12/TiO2
Follow the steps below preparation：
1) under room temperature, butyl titanate is placed in appropriate absolute ethyl alcohol, stir and is sufficiently mixed 1h；Then will
CH3COOLi·2H2O is dissolved in a small amount of deionized water, fully after dissolving, is added dropwise in above-mentioned solution, under drying condition, instead
10-12h is answered, milky reaction solution (CH in the process is obtained3COOLi·2H2Two kinds of raw materials of O and butyl titanate are according to molar ratio Li/
Ti=4:5~5.5 carry out dispensing)；
2) above-mentioned milky reaction solution is placed under 90 DEG C of equal tepidariums and reacts 1h；Then, it is dried in vacuo 6- in 70-80 DEG C
8h obtains intermediate product presoma；
3) intermediate product presoma is placed in air atmosphere, calcines 6-7h in 590-600 DEG C, cools to room temperature with the furnace,
Grinding, obtains intermediate product Li4Ti5O12/TiO2。
A kind of 2 lithium ion battery negative material Li of embodiment4Ti5O12/TiO2The intermediate product Li of/Ag4Ti5O12/TiO2
With embodiment 1, the calcination temperature only changed the step 3) is method：In 690-700 DEG C of calcining.
A kind of 3 lithium ion battery negative material Li of embodiment4Ti5O12/TiO2The intermediate product Li of/Ag4Ti5O12/TiO2
With embodiment 1, the calcination temperature only changed the step 3) is method：In 790-800 DEG C of calcining.
A kind of 4 lithium ion battery negative material Li of embodiment4Ti5O12/TiO2/Ag
Follow the steps below preparation：
1) under room temperature, butyl titanate is placed in appropriate absolute ethyl alcohol, stir and is sufficiently mixed 1h；Then will
CH3COOLi·2H2O is dissolved in a small amount of deionized water, fully after dissolving, is added in above-mentioned solution, under drying condition, reacts 10-
12h obtains milky reaction solution (CH in the process3COOLi·2H2Two kinds of raw materials of O and butyl titanate are according to molar ratio Li/Ti=4:
5~5.5 carry out dispensing)；
2) milky white solution is placed under 90 DEG C of equal tepidariums and reacts 1h；Then, it is dried in vacuo 6- in 70-80 DEG C
8h obtains intermediate product presoma；
3) the product presoma is placed in air atmosphere, 690-700 DEG C of calcining 6-7h cools to room temperature with the furnace, grind
Mill, obtains intermediate product Li4Ti5O12/TiO2。
4) appropriate AgNO at room temperature, is taken3With made Li4Ti5O12/TiO2In deionized water, after ultrasonic disperse 2h, 70-
80 DEG C of vacuum drying 6-8h, obtain target product precursor powder；It then grinds, 500 DEG C of calcinings in Muffle furnace under air atmosphere
2h obtains Li4Ti5O12/TiO2(wherein Ag is to Li for/Ag target products4Ti5O12/TiO2Mass percent be 3wt%).
A kind of 5 lithium ion battery negative material Li of embodiment4Ti5O12/TiO2/Ag
Method is with embodiment 4, and Ag is to Li in only changing the step 4)4Ti5O12/TiO2Mass percent be 5wt%.
A kind of 6 lithium ion battery negative material Li of embodiment4Ti5O12/TiO2/Ag
Method is with embodiment 4, and Ag is to Li in only changing the step 4)4Ti5O12/TiO2Mass percent be 8wt%.
Embodiment 7 detects
The intermediate product Li that embodiment 1,2 and 3 is obtained4Ti5O12/TiO2And the target production that embodiment 4,5 and 6 obtains
Object Li4Ti5O12/TiO2/ Ag carries out XRD characterization respectively, as a result as shown in Figure 1 and Figure 2.
As seen from Figure 1, the intermediate product that embodiment 1-3 is obtained, is spinel-type Li4Ti5O12With Rutile-TiO2's
Composite L i4Ti5O12/TiO2, without other impurity in intermediate product；Improve calcination temperature, the crystallization of respective material simultaneously
Degree also enhances.
From Figure 2 it can be seen that the target product that embodiment 4-6 is obtained, is Li4Ti5O12/TiO2With the composite material of metal Ag,
There is no the presence of other not pure phases in product, this illustrates that the addition of Ag does not change Li4Ti5O12/TiO2Agent structure, and
With the raising of silver-colored additive amount, the characteristic peak of metal Ag is remarkably reinforced.
8 contrast experiment one of embodiment
For the bought LTO materials of embodiment 1-3 resulting materials and common market, using it as cell negative electrode material,
Lithium piece is used as to electrode, is assembled into button cell, is carried out electrochemical property test to it, as a result see
Table 1.
The different negative material chemical properties of table 1 compare (charge-discharge magnification 1C)
By above studies have shown that compared to common LTO negative materials, when calcination temperature is 690-700 DEG C in gained
Between product Li4Ti5O12/TiO2Specific capacity highest, reason is the height of calcination temperature, has very to Product samples crystallite dimension
Big decisive action, 590-600 DEG C of calcination temperature is relatively low, and the crystallinity of intermediate product is relatively low, and 790-800 DEG C
The product of calcining may be because higher temperature makes the particle diameter distribution of sample tend to become larger, and lithium ion exists in structure
Li4Ti5O12/TiO2It inlays in structure and increases with deintercalation difficulty, ionic conductivity declines, so as to cause product chemical property phase
To declining, therefore intermediate product Li4Ti5O12/TiO2Optimum calcinating temperature be 690-700 DEG C.
9 contrast experiment two of embodiment
For the target product Li of three kinds of difference Ag contents obtained by embodiment 4-64Ti5O12/TiO2/ Ag makees it respectively
For cell negative electrode material, lithium piece is used as to electrode, is assembled into button cell, carries out electrochemical property test to it, the results are shown in Table
2。
The different negative material chemical properties of table 2 compare (charge-discharge magnification 1C)
By above studies have shown that compared to intermediate product Li4Ti5O12/TiO2Negative material, the method for the present invention synthesis
Li4Ti5O12/TiO2The chemical property of/Ag nanocomposites is improved significantly, and with the increase of Ag dopings,
Negative material Li synthesized by the method for the present invention4Ti5O12/TiO2The chemical property of/Ag first improves to be weakened afterwards, and can be seen that
Ag is to Li4Ti5O12/TiO2Mass percent obtained Li when being 5wt%4Ti5O12/TiO2/ Ag negative materials, electrification
Learn the negative material that performance is substantially better than gained after other two kinds of doping Ag.Therefore it is preferred that Ag is to Li4Ti5O12/TiO2Quality percentage
Than should be 5wt%.
In conclusion present embodiment provides a kind of lithium ion battery negative material Li4Ti5O12/TiO2/ Ag's is simple
Preparation method is keeping Li4Ti5O12Under the premise of good characteristic, a small amount of TiO is added2, enhance the storage performance of lithium ion；
Meanwhile the shortcomings that in order to improve its low conductivity, it introduces metal Ag and is doped modification, improve the electrochemical properties of sample,
And influence of the Ag dopings to product characteristics is investigated.The cathode material preparation method that this embodiment is provided is simple, system
The negative material Li obtained4Ti5O12/TiO2/ Ag chemical properties are preferable, are advantageously implemented lithium ion battery large-scale application.
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 lithium ion battery negative material Li4Ti5O12/TiO2The preparation method of/Ag, which is characterized in that including walking as follows
Suddenly：
1）Under room temperature, butyl titanate is placed in absolute ethyl alcohol, stirs and be sufficiently mixed 1h, obtains solution A；Then will
CH3COOLi·2H2O is dissolved in deionized water, fully after dissolving, obtains CH3COOLi·2H2O aqueous solutions, by CH3COOLi·2H2O
Aqueous solution is added in solution A, under drying condition, is reacted 10-12h, is obtained milky reaction solution；
2）It will be reacted under the tepidariums such as milky reaction solution is placed in；Then, it is dried in vacuo 6-8h in 70-80 DEG C, obtains intermediate product
Presoma；
3）Intermediate product presoma is placed in air atmosphere, 690-700 DEG C of calcining 6-7h cools to room temperature with the furnace, grind, obtain
Intermediate product Li4Ti5O12 /TiO2；
4）At room temperature, appropriate AgNO is taken3With made intermediate product Li4Ti5O12 /TiO2In deionized water, after ultrasonic disperse,
It is dried in vacuo 6-8h in 70-80 DEG C, obtains powdered target product precursor；It then grinds, under air atmosphere 500 in Muffle furnace
DEG C calcining 2h, obtain target product Li4Ti5O12/TiO2/Ag ；Ag is to Li4Ti5O12/TiO2Mass percent be 3-8wt%.
2. preparation method described in accordance with the claim 1, it is characterised in that：Step 1）Middle CH3COOLi·2H2Four fourth of O and metatitanic acid
Ester is according to molar ratio Li：Ti=4:5 ~ 5.5 carry out dispensing.
3. preparation method described in accordance with the claim 1, it is characterised in that：The step 1）It is middle by CH3COOLi·2H2O is water-soluble
Liquid is added in a manner of being added dropwise in solution A.
4. preparation method described in accordance with the claim 1, it is characterised in that：The step 1）Middle stirring is magnetic agitation.
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| CN101847717A (en) * | 2010-05-27 | 2010-09-29 | 合肥工业大学 | Preparation method of lithium titanate composite negative electrode materials used by lithium ion batteries |
| CN102324511A (en) * | 2011-10-09 | 2012-01-18 | 北京科技大学 | Preparation method for lithium ion battery composite cathode material |
| CN102386385A (en) * | 2011-10-09 | 2012-03-21 | 北京科技大学 | Preparation method of Li4Ti5O12-TiO2 composite electrode material |
| CN102610824A (en) * | 2012-03-26 | 2012-07-25 | 上海大学 | Preparation method of lithium titanate (Li4Ti5O12)/Ag composite lithium-ion negative electrode materials |
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| TWI441779B (en) * | 2010-12-20 | 2014-06-21 | Ind Tech Res Inst | Material of phosphorus-doped lithium titanium oxide with spinel structure and method of manufacturing the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101847717A (en) * | 2010-05-27 | 2010-09-29 | 合肥工业大学 | Preparation method of lithium titanate composite negative electrode materials used by lithium ion batteries |
| CN102324511A (en) * | 2011-10-09 | 2012-01-18 | 北京科技大学 | Preparation method for lithium ion battery composite cathode material |
| CN102386385A (en) * | 2011-10-09 | 2012-03-21 | 北京科技大学 | Preparation method of Li4Ti5O12-TiO2 composite electrode material |
| CN102610824A (en) * | 2012-03-26 | 2012-07-25 | 上海大学 | Preparation method of lithium titanate (Li4Ti5O12)/Ag composite lithium-ion negative electrode materials |
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