CN102637864A - Lanthanum-doped lithium titanate cathode material and preparation method thereof - Google Patents
Lanthanum-doped lithium titanate cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a lanthanum-doped lithium titanate cathode material and a preparation method thereof. The molecular formula of the lanthanum-doped lithium titanate cathode material is LaxLi4-xTi5O12, wherein x is more than 0 and less than or equal to 0.1. The invention further discloses a method for preparing the lanthanum-doped lithium titanate cathode material. The method comprises the following steps of: weighing a titanium source, a lithium source and a lanthanum source, uniformly mixing, and drying; and sintering at the temperature of 550-750 DEG C for 3-5 hours, naturally cooling to room temperature, and grinding. In the preparation method provided by the invention, reactants have low prices, the melting point or decomposing temperature is low, and a low-temperature reaction is easy to undergo. The reaction temperature is low so as to contribute to controlling the appearance and size of the lanthanum-doped lithium titanate cathode material, and crystal grains can be refined by doping trace rare earth lithium, so that the electrochemical performance of lanthanum-doped lithium titanate is improved; compared with non-doped lithium titanate, the prepared lanthanum-doped lithium titanate has the advantages that: the electric conductivity is increased by two orders of magnitude; the prepared lanthanum-doped lithium titanate has superior cycle performance and rate capability without coating carbon on the surface; and the prepared lanthanum-doped lithium titanate is the lanthanum-doped lithium titanate cathode material which has superior high-temperature property and low-temperature property.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, relate to lithium titanate anode material of a kind of lanthanum that mixes and preparation method thereof.
Background technology
Spinelle Li
4Ti
5O
12Embed and deviate from the process to keep good structural stability at lithium ion, lattice constant does not change basically, is a kind of " zero strain " insert type lithium ion battery negative material, has excellent cycle performance; Its smooth voltage platform (1.55 V) is higher than the recovery voltage of most of electrolyte and solvent, thereby can not form passivating film at electrode surface.But the electronics of lithium titanate and ionic conductivity are very low, and high-rate discharge ability is relatively poor, often need improve its chemical property through means such as nanometerization, doping, surface modifications, and not only efficient is low, and effect is obvious inadequately.Explore simple method, realize effective raising of chemical property, help the industrialization and the commercialization of lithium titanate material.
The preparation temperature of lithium titanate is usually above 800 ℃, because the temperature height can cause the loss of lithium, therefore needs to introduce excessive lithium source with the loss in the compensation high-temperature reaction process.The simultaneous temperature height can make lithium titanate crystal grain thick, and pattern and size are difficult to control, cause the lithium titanate chemical property lower.
According to bibliographical information; Do the titanium source through titanium tetrachloride, lanthanum chloride is done the lanthanum source can prepare doping lanthanum lithium titanate, can make the end product composition wayward but form lithium chloride in the course of reaction; And the chloride ion in the product needs to remove through subsequent treatment; Simultaneously product needs through 800 ℃ of high temperature sinterings 16 hours, and electrochemical property test is the result show, doping lanthanum lithium titanate cycle performance and high rate performance through this method preparation are not improved preferably.
In order further to improve the chemical property of lithium titanate, often need carry out follow-up surface bag carbon and handle, both increased cost and consumption, also reduced production efficiency.
Also do not make negative material both at home and abroad at present, constitute the research of full battery aspect with lithium iron phosphate cathode material with lithium titanate.
Summary of the invention
The present invention is for solving the problems of the technologies described above; Lithium titanate anode material of a kind of lanthanum that mixes and preparation method thereof is provided; The doping lanthanum lithium titanate of preparation has excellent cycle performance, high rate performance, high temperature and cryogenic property, and its conductivity more not doped lithium titanate has improved two one magnitude, under the situation that need not wrap carbon, can surpass the advantage of existing lithium titanate material; Simultaneously make negative material with lithium titanate, the full battery that constitutes with lithium iron phosphate cathode material has excellent performance.
To achieve these goals, the present invention adopts following technical scheme.
A kind of lithium titanate anode material of the lanthanum that mixes also contains lanthanum in this lithium titanate material.
A kind of lithium titanate anode material of the lanthanum that mixes, its molecular formula are La
xLi
4-xTi
5O
12, wherein, 0＜x≤0.1.
A kind of method for preparing the lithium titanate anode material of doping lanthanum,
(1) take by weighing titanium source, lithium source and lanthanum source, mix the back oven dry,
(2) after 550-750 ℃ of sintering 3-5 hour, naturally cool to room temperature, grind.
Said titanium source be butyl titanate with or titanium dioxide.
The lanthanum source can be lanthanum nitrate or lanthanum hydroxide.
The lithium source can be in lithium hydroxide, lithium nitrate, lithium carbonate, lithium oxalate, lithium acetate, the lithium stearate etc. one or more.
The invention also discloses a kind of full battery, make negative material to mix the lanthanum lithium titanate, with LiFePO 4 as positive electrode.The invention has the beneficial effects as follows:
1, reactant is cheap, and fusing point or decomposition temperature are low, is easy to carry out low-temp reaction.Wherein the lanthanum nitrate decomposition temperature is 126 ℃, about 400 ℃ of lanthanum hydroxide decomposition temperatures, 471.2 ℃ of lithium hydroxide fusing points; 618 ℃ of lithium carbonate decomposition temperatures, 600 ℃ of lithium nitrate decomposition temperatures, 490 ℃ of lithium oxalate decomposition temperatures; 283 ℃ of lithium acetate fusing points, 220 ℃ of lithium stearate fusing points.Particularly lanthanum nitrate and lithium nitrate are reactant in course of reaction, also are simultaneously the combustion adjuvants of reaction, help reducing the preparation temperature of doping lanthanum lithium titanate.
2, low pattern and the size that helps controlled doping lanthanum lithium titanate of reaction temperature, and the doping of trace rare-earth lanthanum also can crystal grain thinning, thereby improves the chemical property of doping lanthanum lithium titanate;
3, the doping lanthanum lithium titanate of preparation need not carry out surface bag carbon and promptly has performance under excellent cycle performance and high rate performance, the especially 10～50C multiplying power and be superior to the top performance reported at present;
The conductivity of the doping lanthanum lithium titanate that 4, prepares more not doped lithium titanate has improved two one magnitude;
5, the doping lanthanum lithium titanate of preparation has excellent high temperature and cryogenic property, still has very excellent performance-40～60 ℃ of temperature ranges, and this temperature range has surpassed the temperature range-20～55 ℃ of report at present, and performance is better;
6, the full battery of the lithium titanate anode material of the doping lanthanum of preparation and lithium iron phosphate cathode material formation has excellent chemical property.
Description of drawings
Fig. 1 is the x-ray diffraction pattern of the lithium titanate anode material of the doping lanthanum that makes of embodiment 1.
Fig. 2 is the field emission Electronic Speculum shape appearance figure of the lithium titanate anode material of the doping lanthanum that makes of embodiment 4.
Fig. 3 is the pictorial diagram of the lithium titanate anode material of the doping lanthanum that makes of embodiment 4.
Fig. 4 is the lithium titanate anode material high rate performance at room temperature of the doping lanthanum that makes of embodiment 1.
Fig. 5 is the high rate performance of lithium titanate anode material under 60 ℃ of temperature of the doping lanthanum that makes of embodiment 1.
Fig. 6 is the cycle performance under the lithium titanate anode material-40 ℃ temperature of the doping lanthanum that makes of embodiment 1.
Fig. 7 is the voltage and the specific capacity relation of the different cycle-indexes of full battery that constitute of lithium titanate anode material and the lithium iron phosphate cathode material of the doping lanthanum that makes of embodiment 2.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described further.
Embodiment 1:
Lithium titanate anode material through lithium hydroxide and butyl titanate and lanthanum nitrate prepared in reaction doping lanthanum.Weigh in the balance and get 1.16 g lithium hydroxides, 0.12 g lanthanum nitrate adds the 10mL deionized water dissolving.The butyl titanate that takes by weighing 10mL (10g) with graduated cylinder carries out titration.Product is heated in heating furnace about 550 ℃, is incubated and closes heating furnace after 8 hours, naturally cools to room temperature, obtains white powder 2.6 g.
X-ray diffraction pattern such as Fig. 1 of the lithium titanate anode material of the doping lanthanum that present embodiment obtains, each diffraction maximum and spinelle Li among the figure
4Ti
5O
12Match, do not have other dephasigns among the figure, be spinel structure.
The battery that doping lanthanum lithium titanate material among the embodiment makes, the normal temperature Performance Detection: under 25 ℃, under 0.1C, 1C, 5C, 10C, 20C, 50C discharge-rate, electrode is discharged and recharged, test its specific capacity, test is ten times under each multiplying power.Test result is as shown in Figure 4.Can find out with La
xLi
4-xTi
5O
12Be the high current capacity conservation rate that the battery of active material has excellence, it is less that specific capacity is influenced by charging and discharging currents.Under the discharge-rate of 1C, 5C, 10C, 20 C, 50 C, 97.5%, 92.4%, 89.9%, 82.3% and 71.5% when capacity can reach 0.1C respectively.It is thus clear that, can obtain to have the lithium titanate material of excellent electrochemical performance through the doping of Rare Earth Lanthanum element
The battery that doping lanthanum lithium titanate material among the embodiment makes, high-temperature behavior detects: under 60 ℃, under 0.1C, 1C, 5C, 10C discharge-rate, electrode is discharged and recharged, test its specific capacity, test is ten times under each multiplying power.Test result is as shown in Figure 5.Can find out with La
xLi
4-xTi
5O
12Be the high temperature high current capacity conservation rate that the battery of active material has excellence, it is less that specific capacity is influenced by charging and discharging currents.Under 60 ℃, under the discharge-rate of 1C, 5C and 10C, 97.8%, 95.8% and 94.7% when capacity can reach 0.1C respectively.It is thus clear that, can obtain to have the lithium titanate material of excellent high-temperature electrochemical properties through the doping of Rare Earth Lanthanum element
The battery that doping lanthanum lithium titanate material among the embodiment makes, cryogenic property detects: under-40 ℃, under the 0.15C discharge-rate, electrode is discharged and recharged, test its specific capacity.Test result is as shown in Figure 6.Can find out with La
xLi
4-xTi
5O
12Be the low temperature capability retention that the battery of active material has excellence, the specific capacity temperature influence is less.Under the discharge-rate of 0.15C, the low temperature capability retention near 100% is arranged, 73.1% when capacity can reach 25 ℃ of following 0.1C after the circulation.It is thus clear that through the doping of Rare Earth Lanthanum element, the lithium titanate material that can obtain to have excellent low temperature electrochemical performance.
Embodiment 2:
Lithium titanate anode material through lithium nitrate and butyl titanate and lanthanum nitrate prepared in reaction doping lanthanum.Weigh in the balance and get 3.93 g lithium nitrates, 0.18 g lanthanum nitrate adds the 30mL dissolve with ethanol.Take by weighing the 10mL butyl titanate with graduated cylinder and carry out titration.Product is heated in heating furnace about 650 ℃, is incubated and closes heating furnace after 3 hours, naturally cools to room temperature.Obtain white powder 2.7 g.
The full battery that doping lanthanum lithium titanate material among the embodiment and lithium iron phosphate cathode material constitute, normal temperature Performance Detection: under 25 ℃, under the 0.1C discharge-rate, battery is discharged and recharged, test its specific capacity.Test result is as shown in Figure 7.Can find out that with doping lanthanum lithium titanate be negative material, LiFePO 4 is that the full battery that positive electrode constitutes has the excellent charging and discharging performance.Under the 0.1C discharge-rate, capacity can reach 122 mAh/g.It is thus clear that, can obtain to have the full battery of excellent electrochemical performance through the doping of Rare Earth Lanthanum element.
Embodiment 3:
Lithium titanate anode material through lithium nitrate, lanthanum nitrate and titanium dioxide prepared in reaction doping lanthanum.Weigh in the balance and get 3.93 g lithium nitrates, 0.18 g lanthanum nitrate, 5.51g titanium dioxide adds in the 30mL ethanol and mixes.Mixture is heated in heating furnace about 700 ℃, is incubated and closes heating furnace after 3 hours, naturally cools to room temperature.Obtain white powder 5.9 g.
Embodiment 4:
Lithium titanate anode material through lithium hydroxide and butyl titanate and lanthanum nitrate prepared in reaction doping lanthanum.Weigh in the balance and get 1.17 g lithium hydroxides, 0.10 g lanthanum nitrate adds the 10mL deionized water dissolving.The butyl titanate that takes by weighing 10mL (10g) with graduated cylinder carries out titration.Product is heated in heating furnace about 550 ℃, is incubated and closes heating furnace after 6 hours, naturally cools to room temperature.Obtain white powder 2.7 g.
Embodiment 5:
Lithium titanate anode material through lithium hydroxide, lanthanum nitrate and butyl titanate prepared in reaction doping lanthanum.Weigh in the balance and get 1.19 g lithium hydroxides, 0.08 g lanthanum nitrate adds the 10mL deionized water dissolving.Take by weighing 10mL (10g) butyl titanate with graduated cylinder and carry out titration.Product is heated in heating furnace about 550 ℃, is incubated and closes heating furnace after 5 hours, naturally cools to room temperature.Obtain white powder 2.6 g.
Embodiment 6:
Lithium titanate anode material through lithium nitrate, lanthanum nitrate and titanium dioxide prepared in reaction doping lanthanum.Weigh in the balance and get 3.90 g lithium nitrates, 0.21 g lanthanum nitrate, 5.51g titanium dioxide adds in the 30mL ethanol and mixes.Mixture is heated in heating furnace about 650 ℃, is incubated and closes heating furnace after 8 hours, naturally cools to room temperature.Obtain white powder 6.0 g.
Though the above-mentioned accompanying drawing specific embodiments of the invention that combines is described; But be not restriction to protection range of the present invention; One of ordinary skill in the art should be understood that; On the basis of technical scheme of the present invention, those skilled in the art need not pay various modifications that creative work can make or distortion still in protection scope of the present invention.
Claims (7)
1. the lithium titanate anode material of the lanthanum that mixes is characterized in that, also contains lanthanum in the said lithium titanate material.
2. the lithium titanate anode material of doping lanthanum as claimed in claim 1 is characterized in that, its molecular formula is La
xLi
4-xTi
5O
12, wherein, 0＜x≤0.1.
3. a method for preparing the lithium titanate anode material of doping lanthanum comprises the steps:
(1) takes by weighing titanium source, lithium source and lanthanum source, mix the back oven dry;
(2) after 550-750 ℃ of sintering 3-5 hour, naturally cool to room temperature, grind.
4. the method for the lithium titanate anode material of preparation doping lanthanum as claimed in claim 3 is characterized in that, said titanium source be butyl titanate with or titanium dioxide.
5. the method for the lithium titanate anode material of preparation doping lanthanum as claimed in claim 3 is characterized in that, said lanthanum source is lanthanum nitrate or lanthanum hydroxide.
6. the method for the lithium titanate anode material of preparation doping lanthanum as claimed in claim 3 is characterized in that, said lithium source is one or more in lithium hydroxide, lithium nitrate, lithium carbonate, lithium oxalate, lithium acetate, the lithium stearate.
7. a full battery is characterized in that, makes negative material to mix the lanthanum lithium titanate, with LiFePO 4 as positive electrode.
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Cited By (9)
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|---|---|---|---|---|
| CN103151508A (en) * | 2013-03-12 | 2013-06-12 | 上海大学 | Lanthanum lithium titanate doped composite negative electrode material of lithium ion battery and preparation method thereof |
| CN103441257A (en) * | 2013-08-12 | 2013-12-11 | 四川大学 | Preparation method for lithium titanate material |
| CN103779549A (en) * | 2012-10-18 | 2014-05-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of lithium ion batteryelectrode material nano lithium titanate with uniformly-dispersed particles |
| CN105449187A (en) * | 2015-12-20 | 2016-03-30 | 华南理工大学 | Preparation method of high-performance co-doped lithium titanate electrode material |
| CN105789607A (en) * | 2016-05-10 | 2016-07-20 | 内蒙古科技大学 | Preparation method of lithium titanate anode material doped with rare earth |
| CN106252644A (en) * | 2016-08-26 | 2016-12-21 | 浙江长兴金太阳电源有限公司 | A kind of preparation method of lithium ion battery thulium doped titanic acid lithium anode material |
| CN109449433A (en) * | 2018-10-31 | 2019-03-08 | 桑顿新能源科技有限公司 | A kind of preparation method of rear-earth-doped metatitanic acid lithium ultrathin nanometer piece negative electrode material |
| CN109742387A (en) * | 2019-01-16 | 2019-05-10 | 中国科学院福建物质结构研究所 | Rear-earth-doped metatitanic acid lithium electrode material and preparation method thereof |
| CN111554906A (en) * | 2020-05-15 | 2020-08-18 | 辽宁石油化工大学 | Lanthanum-doped titanium trioxide-coated co-modified lithium titanate zinc composite material and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103779549A (en) * | 2012-10-18 | 2014-05-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of lithium ion batteryelectrode material nano lithium titanate with uniformly-dispersed particles |
| CN103779549B (en) * | 2012-10-18 | 2015-11-18 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation method of even particulate dispersion lithium ion battery electrode material nano lithium titanate |
| CN103151508A (en) * | 2013-03-12 | 2013-06-12 | 上海大学 | Lanthanum lithium titanate doped composite negative electrode material of lithium ion battery and preparation method thereof |
| CN103151508B (en) * | 2013-03-12 | 2015-10-07 | 上海大学 | Mix composite cathode material for lithium ion cell of lanthanum lithium titanate and preparation method thereof |
| CN103441257A (en) * | 2013-08-12 | 2013-12-11 | 四川大学 | Preparation method for lithium titanate material |
| CN103441257B (en) * | 2013-08-12 | 2015-10-28 | 四川大学 | A kind of preparation method of lithium titanate material |
| CN105449187A (en) * | 2015-12-20 | 2016-03-30 | 华南理工大学 | Preparation method of high-performance co-doped lithium titanate electrode material |
| CN105789607A (en) * | 2016-05-10 | 2016-07-20 | 内蒙古科技大学 | Preparation method of lithium titanate anode material doped with rare earth |
| CN106252644A (en) * | 2016-08-26 | 2016-12-21 | 浙江长兴金太阳电源有限公司 | A kind of preparation method of lithium ion battery thulium doped titanic acid lithium anode material |
| CN109449433A (en) * | 2018-10-31 | 2019-03-08 | 桑顿新能源科技有限公司 | A kind of preparation method of rear-earth-doped metatitanic acid lithium ultrathin nanometer piece negative electrode material |
| CN109742387A (en) * | 2019-01-16 | 2019-05-10 | 中国科学院福建物质结构研究所 | Rear-earth-doped metatitanic acid lithium electrode material and preparation method thereof |
| CN111554906A (en) * | 2020-05-15 | 2020-08-18 | 辽宁石油化工大学 | Lanthanum-doped titanium trioxide-coated co-modified lithium titanate zinc composite material and preparation method thereof |
| CN111554906B (en) * | 2020-05-15 | 2023-03-31 | 辽宁石油化工大学 | Lanthanum-doped and titanium sesquioxide-coated co-modified lithium titanate zinc composite material and preparation method thereof |
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Application publication date: 20120815 |