CN103151506A - Preparation method of nanoscale zirconium-doped lithium titanate material - Google Patents
Preparation method of nanoscale zirconium-doped lithium titanate material Download PDFInfo
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- CN103151506A CN103151506A CN2013100771419A CN201310077141A CN103151506A CN 103151506 A CN103151506 A CN 103151506A CN 2013100771419 A CN2013100771419 A CN 2013100771419A CN 201310077141 A CN201310077141 A CN 201310077141A CN 103151506 A CN103151506 A CN 103151506A
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- zirconium
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- lithium titanate
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a preparation method of a nanoscale zirconium-doped lithium titanate material. Nanoscale lithium titanate is prepared by the method, and simultaneously is modified through doping zirconium. According to the preparation method, chemical components and grain sizes of the lithium titanate are effectively controlled by using hydro-thermal treatment, the temperature during subsequent treatment is greatly reduced, and grains are prevented from being agglomerated; and the preparation method is easy to implement in industry. The lithium titanate is doped with the zirconium in a preparation process, so that the specific discharge capacity of the material is increased at high magnification. Simultaneously, the gas expansion problem existing in the charge-discharge process of lithium titanate batteries is solved to a certain extent. The material prepared by the method has high magnification and high specific capacity and can be applied to the batteries needed for various portable electronic equipment and various electric vehicles.
Description
Technical field
Relate to a kind of nanoscale and mix the preparation method of zirconium lithium titanate material, belong to the electrochemical power source technical field of material.
Background technology
Along with the development of electrokinetic cell, lithium-ion-power cell becomes main product gradually, and lithium ion battery negative material mainly contains carbon-based material, nitride, silica-base material, tin-based material and various novel alloy.Wherein oneself through practical application be mainly carbon-based material, other material many places are in the laboratory research stage.Although carbon negative pole material has had very large improvement at aspects such as security performance, cycle performances, but still have many shortcomings: the current potential of material with carbon element and the current potential of lithium metal are very approaching, when over-charging of battery, lithium can be separated out and form Li dendrite in carbon electrodes, thereby causes short circuit; First charge-discharge efficiency is low, easily reacts with electrolyte; There is obvious voltage delay phenomenon; Charging platform is uneven; Need add anti-flushing device and may be when high temperature thermal runaway etc.
Lithium titanate (Li with spinel structure
4Ti
5O
12) be considered to that one of negative material of application prospect is arranged most.In lithium ion embedded and deviates from process, the lithium titanate with spinel structure unit cell volume was substantially constant, thereby is called as " zero strain " material.Lithium titanate with spinel structure has following advantage as the cathode of lithium battery of a new generation: 1) spinel-type Li
4Ti
5O
12Theoretical specific capacity is 175mAh/g, and actual specific capacity can reach 160-165mAh/g, and concentrates on land regions, and operating voltage near 2.5V, is 2 times of nickel metal hydride battery when forming battery with the 4V positive electrode; 2) spinelle Li
4Ti
5O
12Structure and physico-chemical property are stable, not with electrolyte reaction, good cycle.3) spinel-type Li
4Ti
5O
12Chemical diffusion coefficient at normal temperatures is 2 * 10
-8cm
2/ s than large 1 order of magnitude of carbon negative pole material, discharges and recharges speed faster.These advantages of lithium titanate battery are conducive to it in the application in electric motor car and energy storage field.At present, the lithium-ion-power cell take lithium titanate as negative pole has become both at home and abroad the competitively focus of exploitation.
As lithium ion battery negative material, the intrinsic conductivity of lithium titanate is 10
-9S/cm belongs to typical insulator, poorly conductive, and heavy-current discharge performance is poor.Address this problem, improve its conductivity, realize the high stability of its large current cycle, it is more effective approach that nanometer, doping metals and carbon coat.The unit that is used for the doping vario-property of lithium titanate have: carbon, iron, magnesium, manganese, aluminium, chromium etc., and make each method and mainly contain solid phase method, liquid phase method etc.
What adopted by vast researcher at present is high temperature solid-state method, is lithium salts, ferrous oxide and carbon source or metal oxide are mixed, and calcines stage by stage the synthesizing blender lithium titanate in 700-1000 ℃ under inert atmosphere protection.The advantage of high temperature method is that technique is simple, easily realizes industrialization, but the common mixing of reactant is inhomogeneous, and the product particle is easily grown up.
Liquid phase method comprises sol-gal process, coprecipitation, hydrothermal synthesis method etc.The technological principle of sol-gel method is: iron, lithium organic substance dissolve or hydrolysis, add the compound of doped chemical, form homogeneous mixture or the compound of molecular level, calcine at last to get the nanocrystal product.Sol-gal process has following advantage: 1. good uniformity; 2. purity is high; 3. heat treatment temperature reduction, time shorten; 4. can prepare nano-powder and film; 5. stoichiometric proportion can accurately be controlled.Its major defect: the organic compound cost is higher; Yield poorly; Volatilize a large amount of organic gas; Be difficult to realize industrialization.
Summary of the invention
Defective for the prior art existence, the object of the present invention is to provide a kind of nanoscale to mix the preparation method of zirconium lithium titanate material, be intended to improve the conductivity of material, improve the high rate charge-discharge performance of negative material, to satisfy modern society to the requirement of lithium ion battery applications.
To achieve these goals, the present invention adopts following technical scheme:
A kind of nanoscale is mixed the preparation method of zirconium lithium titanate material, comprises the steps:
1) the titanium source is dispersed in a certain amount of deionized water, is A liquid; The lithium source is dispersed in a certain amount of deionized water, and keeps the ratio nLi:nTi=1:1.0 of both amount of substances ~ 1.2, add zirconium source solution by 1 ‰ ~ 1% of product gross mass, be B liquid;
2) under magnetic agitation, B liquid is slowly added in A liquid, stir 30min; Mixed solution is poured in hydrothermal reaction kettle, then be placed in 120 ~ 200 ℃ of baking ovens and react 5 ~ 48h, preferably react 12 ~ 24h in 140 ~ 160 ℃ of baking ovens.Reaction naturally cools to room temperature after finishing, and then carries out suction filtration, and with deionized water or ethanol washing, 60 ~ 120 ℃ of dryings obtain precursor;
3) with the presoma of gained under protective atmosphere in 600～1000 ℃ of lower sintering 1 ~ 5h, products therefrom is nanoscale and mixes the zirconium lithium titanate material.
The compound of described titanium is a kind of or its combination in titanium sulfate, butyl titanate, isopropyl titanate, metatitanic acid, amorphous titania, anatase titanium dioxide, rutile titanium dioxide.
The compound of described lithium is a kind of or its combination in lithia, lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium chloride, lithium nitrate.
The compound of described zirconium is a kind of or its combination of zirconia, zirconium oxychloride, zirconium nitrate, zirconium sulfate, zirconium hydroxide, oxalic acid zirconium etc.
Compared with prior art, the present invention has advantages of following outstanding:
The present invention adopts is that hydrothermal synthesis method is processed with solid phase and combined, and the titanium source reacts under higher temperatures with the lithium source in solvent, has realized other dispersion of molecular level, and being more evenly distributed of particle makes the size of product can remain on Nano grade.Nano level lithium titanate material is realized ion-exchange simultaneously under the hydro-thermal dynamic environment, react more abundant, heat energy and kinetic energy are converted to the material internal energy, greatly shortened the processing time, improve productive rate, reduced energy resource consumption and cost, simplified process conditions, the raw material range of choice is wide, is easy in industrial enforcement.The present invention's zirconium that adulterates under hydrothermal condition has shortened heat treatment time, the material grains refinement, and even structure is conducive to the migration of lithium ion and moves out.The present invention's zirconium that adulterates has improved the charge-discharge performance of lithium titanate anode electrode material under high magnification, simultaneously the problem of the flatulence of lithium titanate electrode is had some improvement.
Description of drawings
Fig. 1 is the X-ray diffractogram of the prepared material of the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph that the present invention prepares material.
Fig. 3 is the cycle performance curve of the prepared material of embodiment 1 under different multiplying.
Fig. 4 is the first charge-discharge curve of the prepared material of embodiment 1 under the 0.1C multiplying power.
Embodiment
The specific embodiment of the invention, but the invention is not restricted to following examples.
1) the 34ml tetra-n-butyl titanate is dispersed in the 60ml deionized water, is A liquid; 3.8g one hydronium(ion) oxidation lithium is dispersed in the 40ml deionized water, and to keep the ratio of the amount of substance in lithium source and titanium source be n
Li: n
Ti=1:1.11 presses 1% of gross product quality, and adding 1.05ml zirconium ion concentration is the zirconium source solution of 1mol/L, is B liquid;
2) under magnetic agitation, B liquid is slowly added in A liquid, stir 30min; Mixed solution is poured in the pyroreaction still, then be placed in 180 ℃ of baking ovens and react 12h, reaction naturally cools to room temperature after finishing, and then carries out suction filtration, washs to pH=7 with deionized water, and 60 ℃ of dryings obtain presoma;
3) with presoma 750 ℃ of sintering 2h under nitrogen atmosphere of gained, products therefrom is that nanoscale is mixed the zirconium lithium titanate material.
Adopt the Rigaku D of company the max-2550 X-ray diffractometer sample is carried out material phase analysis (200mA goes on foot wide by 0.02 for CuK α radiation, 40kV
o, sweep speed 8/min, sweep limits (2 θ) is 10
o-70
o, as Fig. 1); Adopt its pattern of S-4800 type sem observation, as Fig. 2.
Be that 80:10:10 mixes according to active material, super conductive carbon black (Super P), binding agent Kynoar (PVDF) mass ratio, film into the approximately electrode film of 0.15mm of thickness with the wet film preparing device, 120 ℃ of dryings are 24 hours under vacuum, be cut into slicing machine the electrode slice that diameter is 12mm, weigh and the accurate quality of calculated activity material.As to electrode and reference electrode, Clegard2500 makes barrier film, 1mol/L LiPF with metal lithium sheet
6EC+DMC (volume ratio 1:1) solution be electrolyte, be assembled into 2016 type button cells in being full of the glove box of argon gas.
Cycle performance curve under different multiplying is seen Fig. 3, and the first discharge specific capacity under the 0.1C multiplying power reaches 160mAhg
-1, near theoretical specific capacity.Specific capacity under the 10C multiplying power is 105 mAhg
-1, capability retention is higher.Fig. 4 is the prepared first charge-discharge curve of lithium titanate material under the 0.1C multiplying power, and its charge and discharge platform is obvious.
1) with the amorphous TiO of 10g
2Be dispersed in the 50ml deionized water, be A liquid; The 11.6g lithium acetate is dispersed in the 50ml deionized water, and keeps the ratio n of the amount of substance in lithium source and titanium source
Li: n
Ti=1:1.1 presses 0.1% of product quality, and adding 0.132ml zirconium ion concentration is the zirconium source solution of 1mol/L, is B liquid;
2) under magnetic agitation, B liquid is slowly added in A liquid, stir 30min; Mixed solution is poured in the pyroreaction still, then be placed in 120 ℃ of baking ovens and react 24h, reaction naturally cools to room temperature after finishing, and then carries out suction filtration, and with the deionized water washing, 120 ℃ of dryings obtain presoma;
3) with the presoma of gained under nitrogen atmosphere in 600 ℃ of sintering 5h, products therefrom is that nanoscale is mixed the zirconium lithium titanate material.
Method of testing is consistent with embodiment 1, and the specific discharge capacity under the 0.1C multiplying power reaches 163mAhg
-1, the specific capacity under the 10C multiplying power is 110 mAhg
-1
Embodiment 3
1) the 402g titanium sulfate is dispersed in the 500ml deionized water, is A liquid; The 85g lithium acetate is dispersed in the 500ml deionized water, and keeps the molar ratio n in lithium source and titanium source
Li: n
Ti=1:1.2, adding 5.27ml zirconium ion concentration by 0.5% of product quality is the zirconium source solution of 1mol/L, is B liquid;
2) under magnetic agitation, B liquid is slowly added in A liquid, stir 30min; Mixed solution is poured in the pyroreaction still, then be placed in 200 ℃ of baking ovens and react 12h, reaction naturally cools to room temperature after finishing, and then carries out suction filtration, and with the deionized water washing, 100 ℃ of dryings obtain presoma;
3) with the presoma of gained under nitrogen atmosphere in 1000 ℃ of sintering 1h, products therefrom is that nanoscale is mixed the zirconium lithium titanate material.
Method of testing is consistent with embodiment 1, and the specific discharge capacity under the 0.1C multiplying power reaches 166mAhg
-1, the specific capacity under the 10C multiplying power is 120 mAhg
-1, capability retention is higher.
Embodiment 4
1) the 28.46ml isopropyl titanate is dispersed in the deionized water of 50ml, is A liquid; 6.56g lithium nitrate is dispersed in the 50ml deionized water, and keeps the molar ratio n in lithium source and titanium source
Li: n
Ti=1:1.05 presses 0.7% of product quality, and adding 0.74ml zirconium ion concentration is the zirconium source solution of 1mol/L, is B liquid;
2) under magnetic agitation, B liquid is slowly added in A liquid, stir 30min; Mixed solution is poured in the pyroreaction still, then be placed in 160 ℃ of baking oven 14h reactions, reaction naturally cools to room temperature after finishing, and then carries out suction filtration, and with the deionized water washing, 100 ℃ of dryings obtain presoma;
3) with presoma 700 ℃ of sintering 5h under nitrogen atmosphere of gained, products therefrom is that nanoscale is mixed the zirconium lithium titanate material.
Method of testing is consistent with embodiment 1, and the specific discharge capacity under the 0.1C multiplying power reaches 164mAhg
-1, the specific capacity under the 10C multiplying power is 120 mAhg
-1, capability retention is higher.
Claims (5)
1. the preparation method that nanoscale is mixed the zirconium lithium titanate material, is characterized in that, comprises the steps:
1) the titanium source is dispersed in a certain amount of deionized water, is A liquid; The lithium source is dispersed in a certain amount of deionized water, and keeps the ratio n of both amount of substances
Li: n
Ti=1:1.0 ~ 1.2 add zirconium source solution by 1 ‰ ~ 1% of product gross mass, are B liquid;
2) under magnetic agitation, B liquid is slowly added in A liquid, stir 30min; Mixed solution is poured in hydrothermal reaction kettle, then be placed in 120 ~ 200 ℃ of baking ovens and react 5 ~ 48h, reaction naturally cools to room temperature after finishing, and then carries out suction filtration, and with deionized water or ethanol washing, 60 ~ 120 ℃ of dryings obtain precursor;
3) with the presoma of gained under protective atmosphere in 600～1000 ℃ of lower sintering 1 ~ 5h, products therefrom is nanoscale and mixes the zirconium lithium titanate material.
2. nanoscale according to claim 1 is mixed the preparation method of zirconium lithium titanate material, it is characterized in that, described step 2) in hydrothermal reaction kettle be placed in 140 ~ 160 ℃ of baking ovens and react 5 ~ 24h.
3. nanoscale according to claim 1 is mixed the preparation method of zirconium lithium titanate material, it is characterized in that, described titanium source is a kind of or its combination in titanium sulfate, butyl titanate, isopropyl titanate, metatitanic acid, amorphous titania, anatase titanium dioxide, rutile titanium dioxide.
4. nanoscale according to claim 1 is mixed the preparation method of zirconium lithium titanate material, it is characterized in that, described lithium source is a kind of or its combination in lithia, lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium chloride, lithium nitrate.
5. nanoscale according to claim 1 is mixed the preparation method of zirconium lithium titanate material, it is characterized in that, described zirconium source is a kind of or its combination in zirconia, zirconium oxychloride, zirconium nitrate, zirconium sulfate, zirconium hydroxide, oxalic acid zirconium.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441256A (en) * | 2013-08-12 | 2013-12-11 | 天津巴莫科技股份有限公司 | High-grinding-density lithium titanate preparation method |
| CN103840191A (en) * | 2014-03-24 | 2014-06-04 | 四川兴能新材料有限公司 | Lithium titanate battery electrolyte film-forming additive doped with zirconium by gradients |
| CN104518210A (en) * | 2013-09-27 | 2015-04-15 | 北京当升材料科技股份有限公司 | Preparation method of composite lithium titanate material |
| CN105261749A (en) * | 2015-10-30 | 2016-01-20 | 攀枝花学院 | Method for preparation zirconium-doped lithium titanate through one-step reaction |
| CN105336939A (en) * | 2015-09-30 | 2016-02-17 | 中国科学院过程工程研究所 | Coating modification method of lithium titanate and lithium ion battery thereof |
| CN106654356A (en) * | 2016-11-30 | 2017-05-10 | 浙江超威创元实业有限公司 | Capacitive lithium-ion start-stop battery |
| CN106848292A (en) * | 2016-11-30 | 2017-06-13 | 浙江超威创元实业有限公司 | A kind of capacitor type lithium ion battery |
| CN106992289A (en) * | 2017-04-16 | 2017-07-28 | 合肥国轩高科动力能源有限公司 | A kind of synthetic method of titanium magnesium lithium chromate and its application as lithium ion battery negative material |
| CN107946554A (en) * | 2017-10-26 | 2018-04-20 | 天津普兰能源科技有限公司 | A kind of preparation method of lithium battery lithium titanate anode material |
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| CN102122710A (en) * | 2009-08-18 | 2011-07-13 | 中国科学院成都有机化学有限公司 | Zr-doped lithium titanate electrode material and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441256A (en) * | 2013-08-12 | 2013-12-11 | 天津巴莫科技股份有限公司 | High-grinding-density lithium titanate preparation method |
| CN104518210A (en) * | 2013-09-27 | 2015-04-15 | 北京当升材料科技股份有限公司 | Preparation method of composite lithium titanate material |
| CN104518210B (en) * | 2013-09-27 | 2018-07-03 | 北京当升材料科技股份有限公司 | A kind of preparation method of composite titanic acid lithium material |
| CN103840191A (en) * | 2014-03-24 | 2014-06-04 | 四川兴能新材料有限公司 | Lithium titanate battery electrolyte film-forming additive doped with zirconium by gradients |
| CN105336939A (en) * | 2015-09-30 | 2016-02-17 | 中国科学院过程工程研究所 | Coating modification method of lithium titanate and lithium ion battery thereof |
| CN105261749A (en) * | 2015-10-30 | 2016-01-20 | 攀枝花学院 | Method for preparation zirconium-doped lithium titanate through one-step reaction |
| CN106654356A (en) * | 2016-11-30 | 2017-05-10 | 浙江超威创元实业有限公司 | Capacitive lithium-ion start-stop battery |
| CN106848292A (en) * | 2016-11-30 | 2017-06-13 | 浙江超威创元实业有限公司 | A kind of capacitor type lithium ion battery |
| CN106992289A (en) * | 2017-04-16 | 2017-07-28 | 合肥国轩高科动力能源有限公司 | A kind of synthetic method of titanium magnesium lithium chromate and its application as lithium ion battery negative material |
| CN107946554A (en) * | 2017-10-26 | 2018-04-20 | 天津普兰能源科技有限公司 | A kind of preparation method of lithium battery lithium titanate anode material |
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Application publication date: 20130612 |