CN102956880B - A kind of for the preparation of Li 4ti 5o 12-TiO 2method of nano composite material and products thereof - Google Patents

A kind of for the preparation of Li 4ti 5o 12-TiO 2method of nano composite material and products thereof Download PDF

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CN102956880B
CN102956880B CN201210459950.1A CN201210459950A CN102956880B CN 102956880 B CN102956880 B CN 102956880B CN 201210459950 A CN201210459950 A CN 201210459950A CN 102956880 B CN102956880 B CN 102956880B
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composite material
nano composite
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glycerol
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CN102956880A (en
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薛丽红
严有为
张五星
许超
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Huazhong University of Science and Technology
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Abstract

The invention discloses a kind of for the preparation of Li 4ti 5o 12-TiO 2the method of nano composite material, comprising: ammoniacal liquor and glycerol are mixed, and form clear solution; Organotitanium polymer and LiOH solution is added successively according to certain consumption proportion in this solution; Under the condition of 120 ~ 200 DEG C, hydro-thermal reaction is performed to obtained mixed solution, thus reaction of formation predecessor; And by the heat treatment 2 ~ 5 hours under the condition of 400-800 DEG C of obtained pre-reaction material, obtain Li thus 4ti 5o 12-TiO 2nano composite material.The invention also discloses corresponding product and purposes.By the present invention, can technique simple, save and can obtain nanoscale Li in seedbed 4ti 5o 12-TiO 2composite powder product, and be convenient to Mass Control and be suitable for large-scale mass production; Obtained product grains size is little, epigranular, and possesses the specific capacity of excellent cycle performance, high rate performance and Geng Gao.

Description

A kind of for the preparation of Li 4ti 5o 12-TiO 2method of nano composite material and products thereof
Technical field
The invention belongs to lithium ion battery electrode material field, more specifically, relate to a kind of for the preparation of Li 4ti 5o 12-TiO 2method of nano composite material and products thereof.
Background technology
The Li of spinel structure 4ti 5o 12material has " zero strain ", the advantage such as long circulation life and high security, is one of desirable negative material of power-type lithium ion battery of new generation.But its theoretical specific capacity is low, and electronic conductivity is low, the corresponding high rate capability seriously constraining this material.Improve Li at present 4ti 5o 12the method of charge-discharge magnification performance mainly contains: 1. by doping high volence metal ion or at Li 4ti 5o 12the coated charcoal of particle surface or other high conductivity material, to form the conductive network, finishing etc. that connect active particle material, improve electron conduction ability; 2. the Li of synthesis nano 4ti 5o 12particle, the corresponding contact area increasing electrode material and electrolyte, shortens Li +migration path, increase Li +mobility, and improve ion conductivity; 3. with Large Copacity negative material phase compound, to improve cycle characteristics and the specific capacity of material.
Research shows, TiO 2as a kind of good electrode material, there is higher theoretical specific capacity (335mAh/g), suitable intercalation potential (~ 2V vs.Li/Li+) and less cubical expansivity (3% ~ 4%), and TiO 2the Li of doping 4ti 5o 12there is better circulation and high rate performance.Therefore, if can Li be prepared 4ti 5o 12-TiO 2nano composite material, will there is important scientific meaning and practical value.
Traditional TiO 2li doped 4ti 5o 12preparation method mostly adopt high-temperature solid phase reaction method or sol-gel process.But these major defects existing for existing preparation method are: high, the consuming time length of energy consumption, product is uneven or particle is larger; In addition, its preparation process technique is loaded down with trivial details, and lacks the regulation and control to electrochemical properties, is therefore difficult to realize Large scale processes and produces the wilderness demand meeting energy field.Correspondingly, also exist in the related art preparation Li 4ti 5o 12-TiO 2the method of composite material makes the technical need improved further.
Summary of the invention
For above defect and the technical need of prior art, the object of the present invention is to provide a kind of for the preparation of Li 4ti 5o 12-TiO 2method of nano composite material and products thereof, it is by studying aspects such as key reaction thing and reaction conditions thereof and improve, can technique simple, save and can obtain nanoscale product in seedbed, and be convenient to Mass Control and be suitable for large-scale mass production; Obtained Li 4ti 5o 12-TiO 2nano composite material crystallite dimension is little, epigranular, and possesses the specific capacity of excellent cycle performance, high rate performance and Geng Gao.
According to one aspect of the present invention, provide a kind of for the preparation of Li 4ti 5o 12-TiO 2the method of nano composite material, is characterized in that, the method comprises the following steps:
A ammoniacal liquor and glycerol mix with the volume ratio of 1:1 ~ 1:20 by (), and form clear solution;
B this clear solution mixes with the organotitanium polymer being selected from butyl titanate or isopropyl titanate by () mutually, it is 0.1 ~ 5.0mol titanium atom/L glycerol that the relation wherein in organotitanium polymer between the addition of titanium atom and glycerol meets;
C () prepares LiOH solution, and to be joined by the LiOH solution of respective volume in the mixed solution that step (b) formed according to the ratio of atomic ratio Li:Ti=0.5 ~ 2.0 and mix;
D () performs hydro-thermal reaction 12 ~ 36 hours to the mixed solution that step (c) obtains under the condition of 120 ~ 200 DEG C, obtain pre-reaction material thus;
E pre-reaction material that step (d) obtains by () is heat treatment 2 ~ 5 hours under the condition of 400-800 DEG C after cleaning-drying process, obtains Li thus 4ti 5o 12-TiO 2nano composite material.
By above design, on the one hand owing to adopting the solution of glycerol and ammoniacal liquor as reaction dissolvent, the cyclic chelate effect of glycerol can be utilized so that the formation of control Ti-O-C key, correspondingly realize TiO 2with Li 4ti 5o 12nano combined, but also the chelating membrane of grain surface can be utilized to suppress nuclei growth, thus be conducive to the size reducing crystal grain; On the other hand, by adopting the LiOH solution of above consumption proportion as reactant and mineralizer, fully carrying out of reaction can be promoted, and guarantee the Li smoothly needed for generation 4ti 5o 12-TiO 2nanocomposite.
As further preferably, in step (b), it is 0.5 ~ 2.0mol titanium atom/L glycerol that the relation between the addition of described titanium atom and glycerol meets.
By the consumption proportion between titanium atom and glycerol is specifically defined as above number range further, more contrast test shows, with more high efficiency, above-mentioned consumption proportion can be guaranteed that reaction obtains and include Li simultaneously 4ti 5o 12and TiO 2nano composite material, the product simultaneously obtained shows better in cycle performance, high rate performance and specific capacity.
As further preferably, in step (d), adopt hydrothermal reaction kettle to be used as the container performing described hydro-thermal reaction, and the mixed solution added account for 50% ~ 80% of the volume of this hydrothermal reaction kettle.
By adopting hydrothermal reaction kettle perform hydro-thermal reaction and the volume of added mixed solution is made above restriction, more contrast test shows, can produce suitable air pressure like this in hydrothermal reaction process, promotes the carrying out of hydro-thermal reaction further; In addition, the problem that when added mixed solution can also be avoided very few, product is on the low side, correspondingly enhances productivity.
As further preferably, in step (d), the mixed solution added accounts for 55% ~ 65% of the volume of this hydrothermal reaction kettle.
According to another aspect of the present invention, additionally provide corresponding nano composite material product.
As further preferably, in obtained nano composite material, described Li 4ti 5o 12for spinel structure, described TiO 2for Anatase or Rutile Type.
According to another aspect of the present invention, additionally provide obtained Li 4ti 5o 12-TiO 2nano composite material is preparing the purposes in cathode material of lithium-ion power battery.
Accompanying drawing explanation
Fig. 1 is for the preparation of Li according to the present invention 4ti 5o 12-TiO 2the process chart of nano composite material;
Fig. 2 a is the X-ray diffraction spectrogram of the 1# sample obtained according to the embodiment of the present invention 1;
Fig. 2 b is the scanning electron microscope (SEM) photograph of the 1# sample obtained according to the embodiment of the present invention 1;
Fig. 2 c charges under 1C multiplying power to this 1# sample and respectively with the charging and discharging curve figure discharging obtained under 1C, 2C, 5C, 10C and 20C multiplying power;
Fig. 2 d is to the cycle performance curve chart of this 1# sample under 1C multiplying power;
Fig. 2 e charges under 1C multiplying power to this 1# sample and respectively with the high rate performance curve chart discharged under 1C, 2C, 5C, 10C and 20C multiplying power, wherein each circulation 20 times.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.In addition, if below in described each execution mode of the present invention involved technical characteristic do not form conflict each other and just can mutually combine.
Fig. 1 is for the preparation of Li according to the present invention 4ti 5o 12-TiO 2the process chart of nano composite material.As shown in fig. 1, in order to prepare required nanoscale Li 4ti 5o 12-TiO 2composite material, first, mixes ammoniacal liquor and glycerol with the volume ratio of 1:1 ~ 1:20, and forms clear solution; This clear solution is mixed mutually with the organotitanium polymer being selected from butyl titanate or isopropyl titanate, it is 0.1 ~ 5.0mol titanium atom/L glycerol that relation wherein in organotitanium polymer between the addition of titanium atom and glycerol meets, and is preferably 0.5 ~ 2.0mol titanium atom/L glycerol.
Then, preparation LiOH solution, and the LiOH solution of respective volume to be added in formed mixed solution according to the ratio of atomic ratio Li:Ti=0.5 ~ 2.0 and mix; The mixed solution obtained for example is contained in hydrothermal reaction kettle, and the mixed solution added accounts for 50% ~ 80% of the volume of this hydrothermal reaction kettle, and preferably 55% ~ 65%, and under the condition of 120 ~ 200 DEG C, perform hydro-thermal reaction 12 ~ 36 hours, obtain pre-reaction material thus.
Finally, by obtained pre-reaction material after cleaning-drying process, under the condition of 400-800 DEG C, heat treatment 2 ~ 5 hours, obtains Li thus 4ti 5o 12-TiO 2nano composite material.
Embodiment 1
By 5mL ammoniacal liquor and 20mL glycerol Homogeneous phase mixing, then add the LiOH solution of 10mmol butyl titanate and 40mL 0.225mol/L successively and mix.Transferred to by above-mentioned mixed solution in the hydrothermal reaction kettle of Teflon liner, wherein added mixed solution accounts for the 55%(of hydrothermal reaction kettle volume and volumetric filling ratio is 65%), and at 150 DEG C hydrothermal treatment consists 24h.After completion of the reaction by generated sediment also namely pre-reaction material deionized water with ethanol purge and drying process, then heat treatment 2h at 400 DEG C, obtains 1# sample.
Fig. 2 a is the X-ray diffraction spectrogram of the 1# sample obtained according to the embodiment of the present invention 1.As can be seen from the figure, the characteristic diffraction peak of this 1# sample is except meeting spinel-type Li 4ti 5o 12outside standard spectrogram, have also appeared Detitanium-ore-type TiO 2diffraction maximum, this illustrate embodiment 1 prepare 1# sample by Li 4ti 5o 12with Detitanium-ore-type TiO 2be composited.
The scanning electron microscope (SEM) photograph of the 1# sample that Fig. 2 b obtains for embodiment 1.As can be seen from the figure, the domain size distribution of this 1# sample is comparatively even, and particle size is less, and average grain diameter is at about 20nm, and grain surface is smooth, and pattern is more regular, and crystallinity is better.
The charging and discharging curve of the 1# sample that Fig. 2 c obtains for embodiment 1.During discharge and recharge, sample is except having a pair stable charging/discharging voltage platform at about 1.5V, also occurs a little charging platform at 2.14V place, and this corresponds to Detitanium-ore-type TiO 2intercalation potential.The discharge capacity of sample when the discharge capacity of 1C multiplying power is 159.6mAh/g, 20C is still up to 151.3mAh/g; Simultaneously along with discharge-rate increases to 20C from 1C, its discharge platform voltage only drops to 1.43V from 1.54V, and the polarization of this material is less as seen, is the ideal electrode material doing electrokinetic cell.
Fig. 2 d shows the cycle performance curve of the 1# sample that embodiment 1 obtains, the first discharge specific capacity of this 1# sample under 1C multiplying power is 184.7mAh/g, coulombic efficiency is that under 89.1%, 1C multiplying power, after 100 circulations, specific discharge capacity is 151.7mAh/g, and capability retention is 82.1%.
Fig. 2 e is the high rate performance curve chart to the 1# sample that embodiment 1 obtains.Can find out in figure, this 1# sample high rate performance is very good, and along with the raising of multiplying power, the discharge capacity of test battery decays to some extent, but it is very little to decay, and during 1C, 2C, 5C, 10C, 20C multiplying power discharging, capacity is respectively 157.5,156.1,154.9 and 150.3mAh/g.
Embodiment 2
By 5mL ammoniacal liquor and 20mL glycerol Homogeneous phase mixing, then add the LiOH solution of 15mmol butyl titanate and 30mL1.0mol/L.Transferred to by said mixture in the hydrothermal reaction kettle of Teflon liner, volumetric filling ratio is 55%, hydrothermal treatment consists 36h at 200 DEG C.After completion of the reaction by sediment deionized water and ethanol purge also drying, then heat treatment 5h at 500 DEG C, obtains 2# sample.
The X-ray diffraction spectrogram of the 2# sample that embodiment 2 is obtained and Li 4ti 5o 12, Detitanium-ore-type TiO 2, rutile TiO 2the contrast of standard spectrogram finds: the characteristic diffraction peak of this 2# sample is except meeting spinel-type Li 4ti 5o 12outside standard spectrogram, have also appeared Detitanium-ore-type TiO 2diffraction maximum, this interpret sample is by Li 4ti 5o 12with Detitanium-ore-type TiO 2be composited.
Embodiment 3
By 1mL ammoniacal liquor and 20mL glycerol Homogeneous phase mixing, then add the LiOH solution of 40mmol butyl titanate and 60mL0.67mol/L.Transferred to by said mixture in the hydrothermal reaction kettle of Teflon liner, volumetric filling ratio is 80%, hydrothermal treatment consists 36h at 120 DEG C.After completion of the reaction by sediment deionized water and ethanol purge also drying, then heat treatment 2h at 800 DEG C, obtains 3# sample.
The X-ray diffraction spectrogram of the 3# sample that embodiment 3 is obtained and Li 4ti 5o 12, Detitanium-ore-type TiO 2, rutile TiO 2the contrast of standard spectrogram finds: the characteristic diffraction peak of this 3# sample is except meeting spinel-type Li 4ti 5o 12outside standard spectrogram, have also appeared the diffraction maximum of rutile TiO_2, this interpret sample is composited by Li4Ti5O12 and rutile TiO_2.
Embodiment 4
By 10mL ammoniacal liquor and 10mL glycerol Homogeneous phase mixing, then add the LiOH solution of 50mmol butyl titanate and 30mL0.83mol/L.Transferred to by said mixture in the hydrothermal reaction kettle of Teflon liner, volumetric filling ratio is 50%, hydrothermal treatment consists 12h at 180 DEG C.After completion of the reaction by sediment deionized water and ethanol purge also drying, then heat treatment 2.5h at 600 DEG C, obtains 4# sample.
The X-ray diffraction spectrogram of 4# sample embodiment 4 obtained and Li4Ti5O12, anatase type tio2, rutile TiO_2 standard spectrogram contrast and find: the characteristic diffraction peak of this 2# sample is except meeting spinel-type Li4Ti5O12 standard spectrogram, also occur the diffraction maximum of rutile TiO_2, this interpret sample is composited by Li4Ti5O12 and rutile TiO_2.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (1)

1. one kind for the preparation of Li 4ti 5o 12-TiO 2the method of nano composite material, is characterized in that, the method comprises the following steps:
A ammoniacal liquor and glycerol mix with the volume ratio of 1:1 ~ 1:20 by (), and form clear solution, this clear solution is as reaction dissolvent and utilize the formation of cyclic chelate effect for control Ti-O-C key of glycerol, but also utilize the chelating membrane of grain surface to suppress nuclei growth, thus be conducive to the size reducing crystal grain;
B this clear solution mixes with the Compound Phase being selected from butyl titanate or isopropyl titanate by (), the relation wherein between the addition of titanium atom and glycerol meets and is: the titanium atom adding 0.5mol ~ 2.0mol in often liter of glycerol;
C () prepares LiOH solution as reactant and mineralizer, to be joined by the LiOH solution of respective volume in the mixed solution that step (b) formed, and mix according to the ratio of atomic ratio Li:Ti=0.5 ~ 2.0;
D () loads in the hydrothermal reaction kettle of Teflon liner to the mixed solution that step (c) obtains, the mixed solution added accounts for 55% ~ 65% of this hydrothermal reaction kettle volume, then under the condition of 120 DEG C ~ 200 DEG C, perform hydro-thermal reaction 12 hours ~ 36 hours, obtain pre-reaction material thus;
E pre-reaction material that step (d) obtains by () is heat treatment 2 hours ~ 5 hours under the condition of 400 DEG C ~ 800 DEG C after cleaning-drying process, obtains Li thus 4ti 5o 12-TiO 2nano composite material, wherein at obtained Li 4ti 5o 12-TiO 2in nano composite material, Li 4ti 5o 12for spinel structure, TiO 2for Anatase or Rutile Type.
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CN103346298A (en) * 2013-06-06 2013-10-09 吉林大学 Preparation method for lithium titanate-titanium oxide composite electrode material
CN104201344A (en) * 2014-09-05 2014-12-10 南开大学 Preparation method of copper-doped Li4Ti5O12-TiO2 regulation and control composite material
CN104993107A (en) * 2015-05-27 2015-10-21 辽宁大学 Lithium ion battery cathode material Li4Ti5O12/rutile-TiO2 and preparation method thereof
CN105206815B (en) * 2015-09-28 2017-11-14 清华大学 A kind of carbon coating Li4Ti5O12‑TiO2/ Sn nano composite materials and its preparation and application
CN106887574A (en) * 2017-03-10 2017-06-23 辽宁大学 A kind of preparation method of regular octahedron pattern lithium ion battery negative material
CN108666557A (en) * 2018-05-29 2018-10-16 陕西动力越源科技有限公司 A kind of lithium ion battery Li4Ti5O12With TiO2Composite electrode material and preparation method thereof
CN108933252A (en) * 2018-09-04 2018-12-04 江南大学 Lithium ion battery lithium titanate and composite titania material and preparation method thereof
CN109546102B (en) * 2018-10-18 2021-01-26 北京航空航天大学 Lithium titanate negative electrode material and preparation method thereof

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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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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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