CN105789583A - Lithium ion battery anode material Li4Ti5O12/TiO2/Ag and preparation method thereof - Google Patents
Lithium ion battery anode material Li4Ti5O12/TiO2/Ag and preparation method thereof Download PDFInfo
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Abstract
The invention provides a lithium ion battery anode material Li4Ti5O12/TiO2/Ag and a preparation method thereof. The invention adopts a simple method of hydrolysis assistance and further calcination to prepare a Li4Ti5O12/TiO2 material; then a method of thermally decomposing AgNO3 to deposit metal Ag plus ultrasonic assistance is adopted to produce the target product, Li4Ti5O12/TiO2/Ag composite material. The preparation method provided by the invention is simple and easy to operate, the lithium ion battery anode material prepared by the method is of a nanoparticle structure, and thereby the specific surface area of the material is enlarged; moreover, under the premise of keeping the excellent properties of the spinel type Li4Ti5O12, the lithium ion battery anode material has the advantages of both TiO2 and metal Ag, and thereby the electrochemical property of the Li4Ti5O12/TiO2/Ag as lithium ion battery anode material is further increased.
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 by high multiplying power lithium ion battery is mainly graphite-like material with carbon element, and the maximum problem of such material is that its surface is easily formed Li dendrite in large current charge process, thus having had a strong impact on the performance of material capacity and thus having caused safety issue.Spinel-type Li4Ti5O12(LTO) being a kind of " zero strain " material, this special performance makes it go out in process to have good reversibility at Lithium-ion embeding/embedding；And, Li4Ti5O12There is stable, higher running voltage (about 1.55V, vsLi+/ Li), the generation of this formation that can avoid Li dendrite and SEI film, thus improve battery security.Just because of the two feature, Li4Ti5O12Become the most promising lithium ion battery negative material；But, its low electron conduction and weak lithium ion diffusibility have impact on lithium ion battery high rate capability, and then limit it and apply on a large scale.
So far, researcheres take many measures to improve LTO electronics and ionic conductivity, including nano materials, bulk phase-doped and high conductivity material cladding etc..
In recent years, a few studies person was devoted to development Ag load LTO material, to improve the electron conduction of LTO, and then improves its high rate capability and cycle performance, and achieves good achievement.Meanwhile, Rutile-TiO2Fast at Lithium-ion embeding-deintercalation process medium-rate, there are higher capacity and good cyclical stability.It is reported, for lithium ion battery negative, about Li4Ti5O12/TiO2The research of/Ag composite is seldom reported.
Summary of the invention
It is an object of the invention to provide a kind of lithium ion battery negative material Li4Ti5O12/TiO2/ Ag and preparation method thereof, to provide the preparation of a kind of simple high efficiency method to have the lithium ion battery negative material of excellent properties.
Technical scheme provided by the invention, specifically, a kind of lithium ion battery negative material Li4Ti5O12/TiO2The preparation method of/Ag, comprises the steps:
1) under room temperature condition, butyl titanate is placed in dehydrated alcohol, stirs and be sufficiently mixed 1h, obtaining solution A；Subsequently by CH3COOLi·2H2O is dissolved in a small amount of deionized water, after fully dissolving, is added in above-mentioned solution A, under drying condition, reacts 10-12h, obtains milky reactant liquor；
2) milky reactant liquor is placed in 90 DEG C and waits reaction 1h under tepidarium；Subsequently, in 70-80 DEG C of vacuum drying 6-8h, intermediate product presoma is obtained；
3) intermediate product presoma is placed in air atmosphere, 590-800 DEG C of calcining 6-7h, cool to room temperature with the furnace, grind, obtain intermediate product Li4Ti5O12/TiO2。
4), under room temperature, appropriate AgNO 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；Grind subsequently, under air atmosphere in Muffle furnace 500 DEG C calcining 2h, obtain target product Li4Ti5O12/TiO2/Ag。
Preferably, step 1) in CH3COOLi·2H2O and butyl titanate carry out dispensing according to mol ratio Li:Ti=4:5～5.5.
It is preferred that, step 1) in CH3COOLi·2H2The feed postition of O solution is for being added dropwise over.
It is preferred that, step 1) in stirring for magnetic agitation.
It is preferred that, step 3) in calcining temperature be 690-700 DEG C.
It is preferred that, step 4) in Ag to Li4Ti5O12/TiO2Mass percent be 3-8wt%, be specially 3wt%, 5wt% and 8wt%, thus preferably going out the consumption of best Ag.
Present invention also offers a kind of lithium ion battery negative material Li4Ti5O12/TiO2/ Ag, described negative material is prepared from by any one method above-mentioned.
Lithium ion battery negative material Li provided by the invention4Ti5O12/TiO2/ Ag and preparation method thereof, it adopts the straightforward procedure of hydrolysis auxiliary and calcining further to prepare Li4Ti5O12/TiO2Material；Subsequently, AgNO is adopted again3Thermal decomposition is in the way of deposit metal Ag, and the prepared target product Li of mode of in addition ultrasonic wave added4Ti5O12/TiO2/ Ag composite.Preparation method provided by the invention is easy, easily operate, and the lithium ion battery negative material being prepared from by the method is nano particle structure, increases the specific surface area of material；Keeping spinel-type Li simultaneously4Ti5O12Under the premise of good characteristic, have TiO concurrently2And the advantage of metal Ag, chemical property when further increasing it as lithium ion battery negative material.Lithium ion battery negative material Li prepared by the method4Ti5O12/TiO2/ Ag is advantageously implemented Li4Ti5O12The commercialization of electrode material, thus promoting its large-scale practical application.
Accompanying drawing explanation
Fig. 1 is different temperatures calcining gained intermediate product Li4Ti5O12/TiO2XRD figure；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/TiO2Process the cell negative electrode material Li of gained further4Ti5O12-TiO2The XRD figure of/Ag；Wherein, Ag is to Li4Ti5O12/TiO2Mass percent respectively a, 3wt%；B, 5wt%；C, 8wt%.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further expalined, but is not limited to protection scope of the present invention.
In order to improve the complicated process of preparation existed in the range of application of lithium ion battery negative material and preparation method, the problem such as wayward further, present embodiment provides a kind of lithium ion battery negative material Li4Ti5O12/TiO2The simple preparation method of/Ag, comprises the steps:
1) under room temperature condition, butyl titanate is placed in dehydrated alcohol, stirs and be sufficiently mixed 1h；Subsequently by CH3COOLi·2H2O is dissolved in a small amount of deionized water, after fully dissolving, is added in above-mentioned solution, under drying condition, reacts 10-12h, obtains milky reactant liquor；
2) described milky white solution is placed in 90 DEG C and waits reaction 1h under tepidarium；Subsequently, in 70-80 DEG C of vacuum drying 6-8h, intermediate product presoma is obtained；
3) described product presoma is placed in air atmosphere, 590-800 DEG C of calcining 6-7h, cool to room temperature with the furnace, grind, obtain intermediate product Li4Ti5O12/TiO2。
4), under room temperature, appropriate AgNO 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；Grind subsequently, under air atmosphere in Muffle furnace 500 DEG C calcining 2h, obtain Li4Ti5O12/TiO2/ Ag target product.
Wherein, good chemical property can be presented in order to ensure obtained negative material, in step 1) in select two kinds of raw material Li sources and Ti source, the two is necessary for liquid, it is thus possible to better haptoreaction, therefore need to use anhydrous alcohol solution butyl titanate, and magnetic agitation 1h makes it be sufficiently mixed；To be added dropwise over CH simultaneously3COOLi·2H2O aqueous solution, otherwise the tetrabutyl titanate hydrolysis in ethanol is too fast, makes solution uneven；The CH of usual 0.530-0.550g3COOLi·2H2O needs the deionized water dissolving of about 10-12ml.Considering, experiment dehydrated alcohol used is 17-25ml.
Step 2) milky white solution is fully dry, grind, obtain intermediate product presoma.
Step 3) in air atmosphere, carry out calcining purpose be in that to be converted into presoma under the high temperature conditions intermediate product Li4Ti5O12/TiO2。
Step 4) in select ultrasonic disperse be make Li4Ti5O12/TiO2With AgNO3It is sufficiently mixed；Select 500 DEG C of calcinings, be because AgNO3Heat decomposition temperature be about 440 DEG C, thus reacting decomposition to obtain Ag, and then form target product.
Being the good nanoparticle distribution of dispersibility in order to ensure obtained negative material, thus increasing the specific surface area of material, improving the chemical property of material, it is preferable that two kinds of raw material CH3COOLi·2H2O and butyl titanate carry out dispensing according to mol ratio Li/Ti=4:5～5.5, to guarantee that the intermediate product formed is for Li4Ti5O12/TiO2。
In order to ensure two kinds of raw material CH3COOLi·2H2O and butyl titanate can sufficiently conducted react, and the hydrolysis rate of butyl titanate is also unsuitable too fast, as the improvement of technical scheme, CH3COOLi·2H2The feed postition of O aqueous solution is for being added dropwise over.
Wherein, step 1) in the stirring that relates to, it is preferred to magnetic agitation, such that it is able to better control mixing speed, improve uniformity coefficient, and easy and simple to handle.
Step 3) in calcining temperature be preferably 690-700 DEG C.
Step 4) in Ag to Li4Ti5O12/TiO2Mass percent be 3-8wt%, it is preferred to 5wt%.
Below in conjunction with the preparation method that specific embodiment further illustrates the present invention.
1 one kinds of lithium ion battery negative material Li of embodiment4Ti5O12/TiO2The intermediate product Li of/Ag4Ti5O12/TiO2
It is prepared according to following steps:
1) under room temperature condition, butyl titanate is placed in appropriate dehydrated alcohol, stirs and be sufficiently mixed 1h；Subsequently by CH3COOLi·2H2O is dissolved in a small amount of deionized water, after fully dissolving, is added dropwise in above-mentioned solution, under drying condition, reacts 10-12h, obtains milky reactant liquor (CH in process3COOLi·2H2O and two kinds of raw materials of butyl titanate carry out dispensing according to mol ratio Li/Ti=4:5～5.5)；
2) above-mentioned milky reactant liquor is placed in 90 DEG C and waits reaction 1h under tepidarium；Subsequently, in 70-80 DEG C of vacuum drying 6-8h, intermediate product presoma is obtained；
3) intermediate product presoma is placed in air atmosphere, calcines 6-7h in 590-600 DEG C, cool to room temperature with the furnace, grind, obtain intermediate product Li4Ti5O12/TiO2。
2 one kinds of lithium ion battery negative material Li of embodiment4Ti5O12/TiO2The intermediate product Li of/Ag4Ti5O12/TiO2
Method with embodiment 1, only changes step 3) calcining heat be: in 690-700 DEG C of calcining.
3 one kinds of lithium ion battery negative material Li of embodiment4Ti5O12/TiO2The intermediate product Li of/Ag4Ti5O12/TiO2
Method with embodiment 1, only changes step 3) calcining heat be: in 790-800 DEG C of calcining.
4 one kinds of lithium ion battery negative material Li of embodiment4Ti5O12/TiO2/Ag
It is prepared according to following steps:
1) under room temperature condition, butyl titanate is placed in appropriate dehydrated alcohol, stirs and be sufficiently mixed 1h；Subsequently by CH3COOLi·2H2O is dissolved in a small amount of deionized water, after fully dissolving, is added in above-mentioned solution, under drying condition, reacts 10-12h, obtains milky reactant liquor (CH in process3COOLi·2H2O and two kinds of raw materials of butyl titanate carry out dispensing according to mol ratio Li/Ti=4:5～5.5)；
2) described milky white solution is placed in 90 DEG C and waits reaction 1h under tepidarium；Subsequently, in 70-80 DEG C of vacuum drying 6-8h, intermediate product presoma is obtained；
3) described product presoma is placed in air atmosphere, 690-700 DEG C of calcining 6-7h, cool to room temperature with the furnace, grind, obtain intermediate product Li4Ti5O12/TiO2。
4), under room temperature, appropriate AgNO 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；Grind subsequently, under air atmosphere in Muffle furnace 500 DEG C calcining 2h, obtain Li4Ti5O12/TiO2(wherein Ag is to Li for/Ag target product4Ti5O12/TiO2Mass percent be 3wt%).
5 one kinds of lithium ion battery negative material Li of embodiment4Ti5O12/TiO2/Ag
Method with embodiment 4, only change step 4) in Ag to Li4Ti5O12/TiO2Mass percent be 5wt%.
6 one kinds of lithium ion battery negative material Li of embodiment4Ti5O12/TiO2/Ag
Method with embodiment 4, only change step 4) in Ag to Li4Ti5O12/TiO2Mass percent be 8wt%.
Embodiment 7 detects
The intermediate product Li that embodiment 1,2 and 3 is obtained4Ti5O12/TiO2And the target product Li that embodiment 4,5 and 6 obtains4Ti5O12/TiO2/ Ag carries out XRD sign respectively, and result is as shown in Figure 1 and Figure 2.
As seen from Figure 1, the intermediate product that embodiment 1-3 obtains, it is spinel-type Li4Ti5O12With Rutile-TiO2Composite L i4Ti5O12/TiO2, intermediate product does not have other impurity；Improving calcining heat, the degree of crystallinity of respective material also strengthens simultaneously.
From Figure 2 it can be seen that the target product that embodiment 4-6 obtains, it is Li4Ti5O12/TiO2With the composite of metal Ag, product does not have other not pure phases, this illustrates that the interpolation of Ag does not change Li4Ti5O12/TiO2Agent structure, and along with silver addition raising, the characteristic peak of metal Ag is remarkably reinforced.
Embodiment 8 contrast experiment one
For the bought LTO material of embodiment 1-3 resulting materials and common market, using it as cell negative electrode material, it, as to electrode, being assembled into button cell, is carried out electrochemical property test by lithium sheet, and result is shown in
Table 1.
The different negative material chemical property of table 1 compares (charge-discharge magnification 1C)
Shown by research above, compared to common LTO negative material, gained intermediate product Li when calcining heat is 690-700 DEG C4Ti5O12/TiO2Specific capacity the highest, reason is in that the height of calcining heat, Product samples crystallite dimension there is very big decisive action, the calcining heat of 590-600 DEG C is relatively low, the degree of crystallinity of intermediate product is relatively low, and the product of 790-800 DEG C of calcining is possibly due to higher temperature and makes the particle size distribution of sample tend to become big, in structure, lithium ion is at Li4Ti5O12/TiO2Inlaying in structure and increase with deintercalation difficulty, ionic conductance declines, thus causing product chemical property relative drop, therefore intermediate product Li4Ti5O12/TiO2Optimum calcinating temperature be 690-700 DEG C.
Embodiment 9 contrast experiment two
Target product Li for three kinds of different Ag content of embodiment 4-6 gained4Ti5O12/TiO2/ Ag, using it as cell negative electrode material, it, as to electrode, being assembled into button cell, is carried out electrochemical property test by lithium sheet, and result is in Table 2.
The different negative material chemical property of table 2 compares (charge-discharge magnification 1C)
Shown by research above, compared to intermediate product Li4Ti5O12/TiO2Negative material, the Li of the inventive method synthesis4Ti5O12/TiO2The chemical property of/Ag nano composite material is improved significantly, and along with the increase of Ag doping, the negative material Li synthesized by the inventive method4Ti5O12/TiO2The chemical property of/Ag first improves and weakens afterwards, and can be seen that Ag is to Li4Ti5O12/TiO2The Li obtained when being 5wt% of mass percent4Ti5O12/TiO2/ Ag negative material, its chemical property is substantially better than the negative material of gained after other two kinds doping Ag.Therefore preferably Ag is to Li4Ti5O12/TiO2Mass percent should be 5wt%.
In sum, present embodiment provides a kind of lithium ion battery negative material Li4Ti5O12/TiO2The simple preparation method of/Ag, is keeping Li4Ti5O12Under the premise of good characteristic, add a small amount of TiO2, enhance the memory property of lithium ion；Meanwhile, in order to improve the shortcoming of its low conductivity, introduce metal Ag and carry out doping vario-property, improve the electrochemical properties of sample, and investigated the impact on product characteristics of the Ag doping.The cathode material preparation method that this embodiment provides is simple, the negative material Li prepared4Ti5O12/TiO2/ Ag chemical property is better, is advantageously implemented lithium ion battery large-scale application.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (6)
1. a lithium ion battery negative material Li4Ti5O12/TiO2The preparation method of/Ag, it is characterised in that comprise the steps:
1) under room temperature condition, butyl titanate is placed in dehydrated alcohol, stirs and be sufficiently mixed 1h, obtaining solution A；Subsequently by CH3COOLi·2H2O is dissolved in deionized water, after fully dissolving, obtains CH3COOLi·2H2O aqueous solution, by CH3COOLi·2H2O aqueous solution is added in solution A, under drying condition, reacts 10-12h, obtains milky reactant liquor；
2) will react under the tepidariums such as milky reactant liquor is placed in；Subsequently, in 70-80 DEG C of vacuum drying 6-8h, intermediate product presoma is obtained；
3) intermediate product presoma is placed in air atmosphere, 590-800 DEG C of calcining 6-7h, cool to room temperature with the furnace, grind, obtain intermediate product Li4Ti5O12/TiO2；
4), under room temperature, appropriate AgNO is taken3With made intermediate product Li4Ti5O12/TiO2In deionized water, after ultrasonic disperse, in 70-80 DEG C of vacuum drying 6-8h, obtain Powdered target product precursor；Grind subsequently, under air atmosphere in Muffle furnace 500 DEG C calcining 2h, obtain target product Li4Ti5O12/TiO2/Ag。
2. the preparation method described in claim 1, it is characterised in that: step 1) in CH3COOLi·2H2O and butyl titanate carry out dispensing according to mol ratio Li:Ti=4:5～5.5.
3. the preparation method described in claim 1, it is characterised in that: described step 1) in by CH3COOLi·2H2O aqueous solution is to be added in solution A in the way of being added dropwise over.
4. the preparation method described in claim 1, it is characterised in that: described step 1) in stirring for magnetic agitation.
5. the preparation method described in claim 1, it is characterised in that: described step 3) in calcining temperature be 690-700 DEG C.
6. the preparation method described in claim 1, it is characterised in that: described step 4) in Ag to Li4Ti5O12/TiO2Mass percent respectively 3-8wt%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113380971A (en) * | 2021-06-07 | 2021-09-10 | 吉首大学 | Composite negative electrode material of thin-film lithium ion battery and preparation method thereof |
| CN115832622A (en) * | 2022-01-30 | 2023-03-21 | 北京卫蓝新能源科技有限公司 | High-power, long-cycle and high-safety lithium battery composite diaphragm and preparation method and application thereof |
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