CN103441257A - Preparation method for lithium titanate material - Google Patents

Preparation method for lithium titanate material Download PDF

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Publication number
CN103441257A
CN103441257A CN2013103490027A CN201310349002A CN103441257A CN 103441257 A CN103441257 A CN 103441257A CN 2013103490027 A CN2013103490027 A CN 2013103490027A CN 201310349002 A CN201310349002 A CN 201310349002A CN 103441257 A CN103441257 A CN 103441257A
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lithium
atmosphere
titanium oxide
lithium titanate
nano titanium
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CN103441257B (en
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张云
张萍
李芳芳
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Sichuan University
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Sichuan University
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a preparation method for lithium titanate material with a spinel structure. Aiming at the performance defect of the conventional material, the preparation method dissolves one or more of the compound formed by Ag, Co, Al, Mg, Zn, Ti, Zr, Si and F and nano titania in a dissolvent, which are agitated together with metatitanic acid, a lithium source and a dispersant in a ball grinding manner, and are radiated by ultraviolet; the materials are ground fine, uniformly mixed, dried, and constantly heated for 2-20 h at a temperature within a range of 600-900 DEG C under a certain atmosphere, and cooled to form the lattice-doped lithium titanate material with the spinel structure, and the prepared material has good volume, circulation and rate capability performance.

Description

A kind of preparation method of lithium titanate material
Technical field
The present invention relates to a kind of preparation method of spinel structural lithium titanate material, particularly the preparation method of a kind of high magnification, high cycle performance lithium titanate anode material, belong to field of energy source materials.
Background technology
Along with the development of World Economics, the energy, information, environment have become three large themes of development in science and technology, and wherein energy problem especially is subject to extensive concern all over the world.Lithium rechargeable battery has many advantages such as operating voltage is high, specific energy is high, volume is little, lightweight, the life-span is long, can not only be for miniaturized electronics provides electric energy as mobile phone, notebook computer, portable video camera, and can provide electric energy for mixing electric car and electric automobile.
Spinel-type metatitanic acid carp (Li 4ti 5o 12) as the electrode material of novel energy storage cell, day by day come into one's own, because spinel type lithium titanate crystal structure in lithium ion embedding, de-embedding process can keep the stability of height, lithium ion is all spinel structure before and after embedding, and lattice constant changes very little, change in volume is very little simultaneously, be less than 1%, so Li 4ti 5o 12be called as " zero strain " electrode material.This can be avoided in charge and discharge cycles because the repeatedly flexible of electrode material causes structural deterioration, thereby cycle performance and the useful life of improving electrode has reduced the decay that brings the specific capacity amplitude with the increase of cycle-index, makes Li 4ti 5o 12there is excellent cycle performance.Compare Li with carbon negative pole material 4ti 5o 12equilibrium potential is higher, has avoided the deposition of metal reason, and its platform capacity surpasses 85% of total capacity, and when charging finishes, current potential rises rapidly, and this phenomenon can be used for indication and stops charging, has avoided overcharging.So Li 4ti 5o 12the fail safe of negative pole is higher than carbon negative pole material.Li 4ti 5o 12the large order of magnitude of chemical diffusion coefficient ratio carbon negative pole material, discharge and recharge speed very fast.Lithium titanate is as negative material and LiCoO 2, LiMn 2o 4, LiNiO 2can form lithium ion battery, all-solid-state battery and hybrid super capacitor with active carbon etc., show good application performance.Simultaneously lithium titanate also has the anti-over-charging performance and the advantage such as thermal stability is good, safe, reliability is high, the life-span is long and specific capacity is large, in fields such as electric automobile, energy-storage batteries, is widely used.The synthetic method of lithium titanate is many, and solid reaction process, high-energy ball milling method and sol-gel process are arranged usually.
Solid phase method technique is simple, but properties of product are not ideal enough, generally needs doping vario-property, but, in the doping vario-property process, doped chemical is difficult to evenly mix and causes properties of product unstable; High-energy ball milling method technique is more complicated, is difficult to realize industrial production.It is good that sol-gel process has a chemical uniformity, the chemical purity advantages of higher, but its shortcoming is also apparent: is added with organic compounds and caused the cost rising; In the process of sintering, gel process is the violent process expanded of a volume, so the utilance of reacting furnace is lower; Organic substance produces a large amount of CO in sintering process 2gas; Complex process, be difficult to realize that large-scale industrial production meets the wilderness demand of energy field.
Because the conductivity of lithium titanate itself is very poor, when high power charging-discharging, capacity can not well be brought into play, therefore need to improve its conductivity to its modification by doping, coating, carbon dope etc., thereby improve the rate performance of lithium titanate, and need with low cost.
Summary of the invention
For making up the deficiency of above-mentioned current material, the present invention is to disclosing a kind of new preparation method who prepares spinel structural lithium titanate material, and concrete summary of the invention is as follows:
1, the present invention relates to a kind of method for preparing the lithium titanate with spinel structure negative material of high power capacity, high rate capability and cycle performance excellence;
2, its preparation method is:
(1) after being dissolved in to solvent together with nano titanium oxide, one or more in the compound of Ag, Co, Al, Mg, Zn, Ti, Zr, Si, F carry out UV-irradiation, and with metatitanic acid, exceed metering than ball grinding stirring 0.5-8h together with the lithium source of 3-10% and dispersant, carry out UV-irradiation simultaneously; By levigate and mix after rear drying materials heated at constant temperature 2-20h under 600-900 ℃ and certain atmosphere, obtain having the spinel structural lithium titanate material of impurity after cooling;
(2) described in above-mentioned (1), the compound of Ag, Co, Al, Mg, Zn, Ti, Zr, Si, F is mainly nitrate, fluoride, acetate, oxide or lipoid substance, the 0.05-2% that its addition is product lithium titanate mole metering ratio;
(3) nano titanium oxide described in above-mentioned (1) is Detitanium-ore-type, rutile-type or two kinds of simultaneous duplex grain structures of crystal formation, and the duplex grain structure of 80% Detitanium-ore-type, 20% rutile-type of wherein take is best, and the granularity of nano titanium oxide is 10-100nm; Wherein take below 50nm as best;
(4) ultraviolet lighting described in above-mentioned (1) is hit the intensity of light source and is: 10-100W uviol lamp or high voltage mercury lamp radiation for every 1L solution or slurry, and luminous range is 3-20cm;
(5) described in above-mentioned (1) in nano titanium oxide and metatitanic acid the mol ratio of titanium be: it is 5-100% that nano titanium oxide accounts for titanium source ratio;
(6) lithium source described in above-mentioned (1) for any one or two kinds of in lithium carbonate and lithium hydroxide, take arbitrary ratio mix after the gained mixture as main, mix and be not more than 3% lithium fluoride or lithium nitrate;
(7) described in above-mentioned (1), dispersant is polyvinyl alcohol or polyethylene glycol;
(8) described in above-mentioned (1), solvent comprises water, ethanol, trichloroethanes, isopropyl alcohol, acetone and the aqueous solution thereof;
(9) described in above-mentioned (1), calcination atmosphere is normal air atmosphere, oxygen-enriched atmosphere, nitrogen atmosphere, argon gas atmosphere or hydrogen atmosphere.
The present invention compared with prior art, has the following advantages:
1, the present invention by the photocatalysis of nano titanium oxide will adulterate ion slowly, uniform deposition is in the titanium source, or slowly, uniform deposition in the compound in ,Li source, titanium source, the doping ion particles is tiny, active high, be easy to finally enter into material lattice, and mix evenly.
2, the present invention adopts nano titanium oxide to combine with metatitanic acid, give full play on the one hand the photocatalysis of nano titanium oxide, adopt on the other hand metatitanic acid can reduce production costs and reduce the granularity of lithium titanate, allow doped chemical distribute more even, the doping ion is easy to enter in the lattice of material simultaneously.
3, the present invention adopts stirring, ball milling and ultraviolet lighting to combine, allow batch mixing process, levigate process and chemical decomposition process carry out simultaneously, allow physical process, chemical process and physical and chemical process occur simultaneously, the uniform ion that is conducive to adulterate enters into lattice, can shorten the high temperature generated time in later stage simultaneously.
4, take spinel lithium titanate prepared by the present invention is positive electrode, the lithium sheet is negative material, by conductive agent carbon black (10wt%), binding agent Kynoar (PVDF, N-N-methyl 2-pyrrolidone N-(NMP) solution and above-mentioned positive electrode (85wt%) 5wt%) mix, make slurry, make lithium ion battery, more than under the 0.2C multiplying power, between 2.75 ~ 4.3V, specific discharge capacity reaches 165mAh/g, after 300 circulations, capability retention can reach more than 98%.
5, technique of the present invention is simple to operation, and environmentally friendly, reduces production costs, and is easy to large-scale industrialization production.
The accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 1 prepared material
Fig. 2 is the discharge curve of prepared material in the embodiment of the present invention 2
Fig. 3 is the SEM of prepared material in the embodiment of the present invention 4
Fig. 4 is the charge and discharge cycles curve of prepared material in the embodiment of the present invention 3.
Embodiment
In order better to understand the present invention, below in conjunction with embodiment and accompanying drawing, the present invention will be further explained, (with Li 4ti 5o 12product 100g is prepared burden) but that embodiments of the present invention are not limited to is following several.
Embodiment 1
The preparation method of lithium titanate with spinel structure of the present invention comprises the following steps:
(1) with the titanium source of nano titanium oxide and metatitanic acid mol ratio 1:1, excessive 5% Li 2cO 3for the lithium source, add together in ethanol medium and form the slurry that solid content is 30%, then carry out UV-irradiation after adding mol ratio 0.2% silver nitrate in ball grinding stirring, the time is 5h.
(2) by after the drying materials after above-mentioned processing, under the oxygen atmosphere of oxygen concentration 30% and 800 ℃, calcining 12h, cool to room temperature with the furnace, obtain mixing the spinel lithium titanate material of Ag.
The spinel lithium titanate made of take is positive electrode, the lithium ion battery that the lithium sheet is negative pole assembling carries out charge-discharge test under the 0.2C multiplying power, between 2.75 ~ 4.3V, experimental result shows that specific discharge capacity reaches 165mAh/g, and after 300 circulations, capability retention is higher than 97%.
Embodiment 2
(1) take nano titanium oxide as the titanium source, be distributed in aqueous medium and form the slurry that solid content is 10%, adding 0.05% polyethylene glycol is dispersant, carry out UV-irradiation 2h after adding lithium titanate mol ratio 0.2% aluminum nitrate, 0.2% zirconia in ball grinding stirring, adding by the lithium hydroxide measured than excessive 5% is the lithium source again, the solid content that adds water adjusting slurry is 25%, then continues stirring ball-milling 3h.
(2) by after the drying materials after above-mentioned processing, under nitrogen atmosphere and 900 ℃, calcining 6h, cool to room temperature with the furnace, obtain mixing the spinel lithium titanate material of aluminium and zirconium.
The spinel lithium titanate made of take is positive electrode, the lithium ion battery that the lithium sheet is negative pole assembling carries out charge-discharge test under the 0.2C multiplying power, between 2.75 ~ 4.3V, experimental result shows that specific discharge capacity reaches 159mAh/g, and after 300 circulations, capability retention is higher than 99%.
Embodiment 3
(1) take mole metering is distributed in aqueous medium and forms the slurry that solid content is 10% than 10% nano titanium oxide, carry out UV-irradiation 2h after adding lithium titanate mole metering than 0.2% zinc acetate, 0.5% nano silicon oxide in ball grinding stirring, add again mole metering than 90% metatitanic acid, continue ball grinding stirring and carry out UV-irradiation 1h, last adding again by the lithium source of measuring than excessive 8%, the lithium source consist of the metering of lithium hydroxide and lithium carbonate than for each 50%, the solid content that adds water adjusting slurry is 35%, then continues stirring ball-milling 2h.
(2) by after the drying materials after above-mentioned processing, under argon gas atmosphere and 750 ℃, calcining 15h, cool to room temperature with the furnace, obtain mixing the spinel lithium titanate material of zinc and silicon.
The spinel lithium titanate made of take is positive electrode, the lithium ion battery that the lithium sheet is negative pole assembling carries out charge-discharge test under the 0.2C multiplying power, between 2.75 ~ 4.3V, experimental result shows that specific discharge capacity reaches 163mAh/g, and after 300 circulations, capability retention is higher than 97%.
Embodiment 4
(1) take mole metering is distributed in aqueous medium and forms the slurry that solid content is 20% than 30% nano titanium oxide, 70% metatitanic acid, add lithium titanate mole metering than 1% lithium fluoride, 0.5% nano aluminium oxide, carry out UV-irradiation 2h in ball grinding stirring, last adding again by the lithium source of measuring than excessive 6%, the lithium source consists of mole metering than 10% lithium hydroxide and 90% lithium carbonate, then continues stirring ball-milling 2h.
(2) by after the drying materials after above-mentioned processing, under air atmosphere and 700 ℃, calcining 15h, cool to room temperature with the furnace, obtain mixing the spinel lithium titanate material of zinc and silicon.
The spinel lithium titanate made of take is positive electrode, the lithium ion battery that the lithium sheet is negative pole assembling carries out charge-discharge test under the 0.2C multiplying power, between 2.75 ~ 4.3V, experimental result shows that specific discharge capacity reaches 160mAh/g, and after 300 circulations, capability retention is higher than 95%.

Claims (9)

1. after one or more in the compound of Ag, Co, Al, Mg, Zn, Ti, Zr, Si, F being dissolved in to solvent together with nano titanium oxide, carry out UV-irradiation, and with metatitanic acid, exceed metering than ball grinding stirring 0.5-8h together with the lithium source of 3-10% and dispersant, carry out UV-irradiation simultaneously; By levigate and mix after rear drying materials heated at constant temperature 2-20h under 600-900 ℃ and certain atmosphere, obtain having the spinel structural lithium titanate material of impurity after cooling.
2. described in claim (1), the compound of Ag, Co, Al, Mg, Zn, Ti, Zr, Si, F is mainly nitrate, fluoride, acetate, oxide or lipoid substance, the 0.05-2% that its addition is product lithium titanate mole metering ratio.
3. nano titanium oxide described in claim (1) is Detitanium-ore-type, rutile-type or two kinds of simultaneous duplex grain structures of crystal formation, and the duplex grain structure of 80% Detitanium-ore-type, 20% rutile-type of wherein take is best, and the granularity of nano titanium oxide is 10-100nm; Wherein take below 50nm as best.
4. ultraviolet lighting described in claim (1) is hit the intensity of light source and is: 10-100W uviol lamp or high voltage mercury lamp radiation for every 1L solution or slurry, luminous range is 3-20cm.
Described in claim (1) in nano titanium oxide and metatitanic acid the mol ratio of titanium be: it is 5-100% that nano titanium oxide accounts for titanium source ratio.
Lithium source described in claim (1) for any one or two kinds of in lithium carbonate and lithium hydroxide, take arbitrary ratio mix after the gained mixture as main, mix and be not more than 3% lithium fluoride or lithium nitrate.
7. described in claim (1), dispersant is polyvinyl alcohol or polyethylene glycol.
8. described in claim (1), solvent comprises water, ethanol, trichloroethanes, isopropyl alcohol, acetone and the aqueous solution thereof.
9. described in claim (1), calcination atmosphere is normal air atmosphere, oxygen-enriched atmosphere, nitrogen atmosphere, argon gas atmosphere or hydrogen atmosphere.
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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN104779392A (en) * 2015-04-14 2015-07-15 淄博蓝印化工有限公司 Titanium phosphate lithium doped lithium titanate electrode material and manufacturing method thereof
CN105226263A (en) * 2015-10-20 2016-01-06 四川科能锂电有限公司 The preparation method of lithium titanate
JP2017073265A (en) * 2015-10-07 2017-04-13 株式会社豊田中央研究所 Complex and manufacturing method thereof
CN107324379A (en) * 2017-06-30 2017-11-07 江苏特丰新材料科技有限公司 A kind of high power capacity lithium titanate material preparation method
CN108946799A (en) * 2018-09-26 2018-12-07 山东精工电子科技有限公司 The method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate
CN113264550A (en) * 2021-05-18 2021-08-17 攀枝花学院 Preparation method of lithium titanate negative electrode material

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104779392A (en) * 2015-04-14 2015-07-15 淄博蓝印化工有限公司 Titanium phosphate lithium doped lithium titanate electrode material and manufacturing method thereof
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CN107324379A (en) * 2017-06-30 2017-11-07 江苏特丰新材料科技有限公司 A kind of high power capacity lithium titanate material preparation method
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CN113264550A (en) * 2021-05-18 2021-08-17 攀枝花学院 Preparation method of lithium titanate negative electrode material

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