CN104617273A - Spherical porous lithium titanate/titanium dioxide composite material as well as preparation method and application of composite material - Google Patents
Spherical porous lithium titanate/titanium dioxide composite material as well as preparation method and application of composite material Download PDFInfo
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Abstract
The invention provides a spherical porous lithium titanate/titanium dioxide composite material as well as a preparation method and application of compositematerial. The preparation method comprises the following steps: dissolving a lithium source and a surfactant in anhydrous alcohol, then adding glacial acetic acid and a titanium source inside, mixing uniformly, subsequently atomizing, drying and decomposing to obtain a body; and subsequently calcining at high temperature to obtain the porous spherical lithium titanate/titanium dioxide composite material. Compared with the prior art, the spherical porous lithium titanate/titanium dioxide composite prepared according to the preparation method has the size of 0.2-1 microns and pore size of 15-20 nanometers, has a uniform and perfect spherical shape, and is beneficial totapping and compacting, is of a porous structure is beneficial to the permeation and diffusion of electrolytes andsimultaneously facilitates transferring of lithium ions, and the subsequent screening is not needed due to the size of 0.2-1 microns; moreover, according to the preparation method disclosed by the invention,the requirements on equipment is low, and presintering and mixing are not needed, and the common high-temperature furnace can produce the composite material; and being as an electrode material, the composite material disclosed by the invention has relatively high special capacity reaching 166 mAh/g under 1C rate.
Description
Technical field
The present invention relates to field of lithium ion battery anode, specifically relate to a kind of spherical porous lithium titanate/composite titania material, preparation method and application thereof.
Background technology
Lithium ion battery is for traditional secondary cell, advantage based on himself comprise energy density high, have extended cycle life, concern that good stability, memory-less effect etc. are subject to people day by day, lithium ion has been widely applied in the multiple portable type electronic products such as mobile phone, notebook computer, electric motor car.In recent years, because the environmental consciousness of people is more and more stronger, the application of lithium ion battery has also been extended to the scope of pure power car and hybrid electric vehicle.
At present, business-like lithium ion battery negative material mainly adopts carbon-based material, although material with carbon element is cheap, non-toxic, but itself also exists defect.When carbon-based material is as lithium cell negative pole, the compound formed after inserting lithium differs less than 0.5V with the current potential of lithium, and when over-charging of battery, carbon electrodes easily separates out very active lithium metal, forms dendrite lithium, may pierce through the danger that barrier film causes short circuit.In addition, the cyclical stability of carbon-based material is poor, coulombic efficiency is low first, and also easy and electrolyte is had an effect.These shortcomings are all unfavorable for the stable of battery and safety.
Compared with carbon-based material, lithium titanate material (Li4Ti5O12) then has clear superiority: first, lithium titanate material is zero strain material, before and after discharge and recharge, crystal structure is highly stable, change hardly, the structural deterioration of generation because electrode material is flexible back and forth in charge and discharge process can be avoided, thus there is superior cycle performance; Moreover lithium titanate material has higher ionic diffusion coefficient, an order of magnitude higher than carbon negative pole material usually, and also its thermal stability is fine; Secondly, it has more stable charge and discharge platform, and average voltage platform is 1.56V, and actual specific capacity can reach 165mAh/g (theoretical specific capacity 175mAh/g); Finally, lithium titanate material low price, is easy to preparation, is applicable to commercially producing.Therefore, lithium titanate can as a kind of electrode material of desirable replacement carbon-based material.Meanwhile, through investigation pertinent literature, we find, the chemical property of lithium titanate/composite titania material is better than the lithium titanate material of pure phase, has higher specific capacity, and spherical loose structure lithium titanate/composite titania material yet there are no report.
Summary of the invention
The object of the present invention is to provide a kind of spherical porous lithium titanate/composite titania material and preparation method thereof, adopt spraying dry assisted synthesizing method, the spherical porous lithium titanate/composite titania material prepared has the features such as height ratio capacity, high rate capability and long-life.
Present invention also offers a kind of application of spherical porous lithium titanate/composite titania material.
Spherical porous lithium titanate/the composite titania material of one provided by the invention, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
The preparation method of a kind of spherical porous lithium titanate/composite titania material provided by the invention, comprises the following steps:
(1), by lithium source and surfactant be dissolved in absolute ethyl alcohol, then add glacial acetic acid and titanium source, ultrasonicly to mix, obtain mixed solution;
(2), by step (1) gained mixed solution carry out atomizer atomization, decomposed by high temperature furnace drying, collect spherical precursor;
(3), by presoma collected in step (2) in air atmosphere, after high-temperature calcination, naturally cool to room temperature, porous spherical lithium titanate/composite titania material can be obtained.
In the mixed solution that step (1) obtains, in mixed solution, the molar ratio of lithium source, titanium source, surfactant, ethanol, each material of acetic acid is: 0.1-1:1:0.005-0.03:120-250:0.6-7, lithium source is selected from lithium nitrate, lithium chloride, lithium acetate, titanium source is selected from butyl titanate (TBOT), described surfactant be P123, F127, CTAB any one, the glacial acetic acid added is intended to control the hydrolysis of butyl titanate.
Described in step (2), the power of atomizer is 35W, and frequency is 1.7MHz.
It is 450-480 DEG C that furnace temperature is decomposed in the drying of high temperature furnace described in step (2).
Described in step (3), high-temperature calcination condition is: programming rate 5 DEG C/min, at 600 DEG C of calcining 4-8h.
The application of a kind of spherical porous lithium titanate/composite titania material provided by the invention, as the application of electrode material.
Spherical porous for gained lithium titanate/composite titania material, super P-Li conductive black and PVDF adhesive are fully ground according to the ratio of 75:15:10 respectively, and furnishing uniform sizing material, on coating Cu paper tinsel, dry, compacting.2032 type button cell (H are assembled in the glove box of high-purity argon gas (purity is greater than 99.99%) atmosphere
2o content is less than 1ppm, O
2content is less than 3ppm).Wherein metal lithium sheet is as negative pole.
Compared with prior art, spherical porous lithium titanate/composite titania material prepared by the present invention, be of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer, spherical even perfection, is conducive to jolt ramming and compacting; Its loose structure, is conducive to infiltration and the diffusion of electrolyte, is convenient to the transmission of lithium ion simultaneously; Size at 0.2 ~ 1 micron, without the need to follow-up screening; And preparation method prepared by the present invention is simple, and equipment requirement is low, without the need to pre-burning and batch mixing, namely common high temperature furnace meets produces; As electrode material, have higher specific capacity, under 1C multiplying power, capacity is up to 166mAh/g.
Accompanying drawing explanation
Fig. 1 is scanning electron microscopy (SEM) photo of the spherical porous lithium titanate/composite titania material of embodiment 1 gained;
Fig. 2 is X-ray powder diffraction (XRD) style of the spherical porous lithium titanate/composite titania material of embodiment 1 gained;
Fig. 3 is the charging and discharging curve of 2032 type button cells in 1C multiplying power of the spherical porous lithium titanate of embodiment 1 and embodiment 5 gained/composite titania material assembling;
Fig. 4 is the capacity circulating figure of 2032 type button cells under 2C multiplying power of the spherical porous lithium titanate/composite titania material of embodiment 1 and embodiment 5 gained and comparative example 1 and comparative example 2 gained spherical lithium titanate/composite titania material assembling.
Embodiment
Embodiment 1
A kind of spherical porous lithium titanate/composite titania material, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
A preparation method for spherical porous lithium titanate/composite titania material, comprises the following steps:
(1) 0.1544 gram of LiNO, is taken
3be dissolved in 20mL ethanolic solution with 0.25 gram of P123, then in gained solution, add 0.5mL glacial acetic acid solution and 1mL butyl titanate (TBOT) solution, mix under ultrasonic;
(2), step (1) gained reactant mixed solution is atomized in atomizer, simultaneously in vacuum under the drainage of vacuum pump, fog is imported in high temperature furnace through grass tube, at high temperature furnace 480 DEG C, dry decomposition, obtains solid product and spherical precursor;
(3), by collect powder in atmosphere 600 DEG C calcining 8 hours, heating rate 5 DEG C/min.
An application for spherical porous lithium titanate/composite titania material, as the application of electrode material.
Embodiment 2
A kind of spherical porous lithium titanate/composite titania material, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
A preparation method for spherical porous lithium titanate/composite titania material, comprises the following steps:
(1) 0.0193 gram of LiNO, is taken
3be dissolved in 20mL ethanolic solution with 0.032 gram of F127, then in gained solution, add 0.5mL glacial acetic acid solution and 0.9mL TBOT solution, mix under ultrasonic;
(2), by gained solution atomizer in step (1) be atomized, decompose (furnace temperature 480 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 8 hours, heating rate 5 DEG C/min.
An application for spherical porous lithium titanate/composite titania material, as the application of electrode material.
Embodiment 3
A kind of spherical porous lithium titanate/composite titania material, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
A preparation method for spherical porous lithium titanate/composite titania material, comprises the following steps:
(1) 0.0965 gram of LiNO, is taken
3be dissolved in 20mL ethanolic solution with 0.10 gram of P123, then in gained solution, add 0.5mL glacial acetic acid solution and 1mL TBOT solution, mix under ultrasonic;
(2), by gained solution atomizer in step (1) be atomized, decompose (furnace temperature 480 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 8 hours, heating rate 5 DEG C/min.
An application for spherical porous lithium titanate/composite titania material, as the application of electrode material.
Embodiment 4
A kind of spherical porous lithium titanate/composite titania material, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
A preparation method for spherical porous lithium titanate/composite titania material, comprises the following steps:
(1) 0.1158 gram of LiNO, is taken
3be dissolved in 20mL ethanolic solution with 0.50 gram of P123, then in gained solution, add 1.0mL glacial acetic acid solution and 0.9mL TBOT solution, mix under ultrasonic;
(2), by gained solution atomizer in step (1) be atomized, decompose (furnace temperature 480 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 8 hours, heating rate 5 DEG C/min.
An application for spherical porous lithium titanate/composite titania material, as the application of electrode material.
Embodiment 5
A kind of spherical porous lithium titanate/composite titania material, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
A preparation method for spherical porous lithium titanate/composite titania material, comprises the following steps:
(1) 0.1738 gram of LiNO, is taken
3be dissolved in 20mL ethanolic solution with 0.25 gram of P123, then in gained solution, add 0.5mL glacial acetic acid solution and 1mL TBOT solution, mix under ultrasonic;
(2), by gained solution atomizer in step (1) be atomized, decompose (furnace temperature 480 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 8 hours, heating rate 5 DEG C/min.
An application for spherical porous lithium titanate/composite titania material, as the application of electrode material.
Embodiment 6
A kind of spherical porous lithium titanate/composite titania material, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
A preparation method for spherical porous lithium titanate/composite titania material, comprises the following steps:
(1) 0.1931 gram of LiNO, is taken
3be dissolved in 40mL ethanolic solution with 0.015 gram of CTAB, then in gained solution, add 0.5mL glacial acetic acid solution and 1mL TBOT solution, mix under ultrasonic;
(2), by gained solution atomizer in step (1) be atomized, decompose (furnace temperature 480 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 8 hours, heating rate 5 DEG C/min.
An application for spherical porous lithium titanate/composite titania material, as the application of electrode material.
Embodiment 7
A kind of spherical porous lithium titanate/composite titania material, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
A preparation method for spherical porous lithium titanate/composite titania material, comprises the following steps:
(1) 0.1544 gram of LiNO, is taken
3be dissolved in 20mL ethanolic solution with 0.25 gram of P123, then in gained solution, add 0.5mL glacial acetic acid solution and 1mL TBOT solution, mix under ultrasonic;
(2), by gained solution atomizer in step (1) be atomized, decompose (furnace temperature 480 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 12 hours, heating rate 5 DEG C/min.
An application for spherical porous lithium titanate/composite titania material, as the application of electrode material.
Embodiment 8
A kind of spherical porous lithium titanate/composite titania material, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
A preparation method for spherical porous lithium titanate/composite titania material, comprises the following steps:
(1), take 0.1478 gram of lithium acetate and 0.25 gram of P123 is dissolved in 20mL ethanolic solution, then add 0.1mL glacial acetic acid solution and 1mL TBOT solution in gained solution, mix under ultrasonic;
(2), by gained solution atomizer in step (1) be atomized, decompose (furnace temperature 480 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 4 hours, heating rate 5 DEG C/min.
An application for spherical porous lithium titanate/composite titania material, as the application of electrode material.
Embodiment 9
A kind of spherical porous lithium titanate/composite titania material, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
A preparation method for spherical porous lithium titanate/composite titania material, comprises the following steps:
(1) 0.1544 gram of LiNO, is taken
3be dissolved in 20mL ethanolic solution with 0.25 gram of P123, then in gained solution, add 1.0mL glacial acetic acid solution and 1mL TBOT solution, mix under ultrasonic;
(2), by gained solution atomizer in step (1) be atomized, decompose (furnace temperature 450 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 8 hours, heating rate 5 DEG C/min.
An application for spherical porous lithium titanate/composite titania material, as the application of electrode material.
Embodiment 10
A kind of spherical porous lithium titanate/composite titania material, is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
A preparation method for spherical porous lithium titanate/composite titania material, comprises the following steps:
(1), take 0.095 grams lithium chloride and 0.25 gram of P123 is dissolved in 20mL ethanolic solution, then add 1.0mL glacial acetic acid solution and 1mL TBOT solution in gained solution, mix under ultrasonic;
(2), by gained solution atomizer in step (1) be atomized, decompose (furnace temperature 450 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 8 hours, heating rate 5 DEG C/min.
An application for spherical porous lithium titanate/composite titania material, as the application of electrode material.
Comparative example 1
(1) 0.1544 gram of LiNO, is taken
3be dissolved in 20mL ethanolic solution, then in gained solution, add 0.5mL glacial acetic acid solution and 1mL butyl titanate (TBOT) solution, mix under ultrasonic;
(2), by gained solution atomizer in step (1) be atomized, decompose (furnace temperature 480 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 8 hours, heating rate 5 DEG C/min.
An application for spherical lithium titanate/composite titania material, as the application of electrode material.
Comparative example 2
(1) 0.1738 gram of LiNO, is taken
3be dissolved in 20mL ethanolic solution, then in gained solution, add 0.5mL glacial acetic acid solution and 1mL TBOT solution, mix under ultrasonic;
(2), by gained solution atomizer in step one be atomized, decompose (furnace temperature 480 DEG C) by high temperature furnace drying, finally collect powder particle;
(3), by collect powder in atmosphere 600 DEG C calcining 8 hours, heating rate 5/min.
An application for spherical lithium titanate/composite titania material, as the application of electrode material.
2032 type button cells of spherical porous lithium titanate prepared by embodiment 1 and embodiment 5/composite titania material assembling, 1C multiplying power charging and discharging curve as shown in Figure 3, and the capacity circulating figure of the 2032 type button cells assembled with spherical lithium titanate/composite titania material prepared by comparative example 1 and comparative example 2 under 2C multiplying power is as shown in Figure 4.
Claims (10)
1. spherical porous lithium titanate/composite titania material, is characterized in that, described spherical porous lithium titanate/composite titania material is spherical porous structure, is of a size of 0.2 ~ 1 micron, aperture 15 ~ 20 nanometer.
2. a preparation method for spherical porous lithium titanate/composite titania material according to claim 1, comprises the following steps:
(1), by lithium source and surfactant be dissolved in absolute ethyl alcohol, then add glacial acetic acid and titanium source, ultrasonicly to mix, obtain mixed solution;
(2), by step (1) gained mixed solution carry out atomizer atomization, decomposed by high temperature furnace drying, collect spherical precursor;
(3), by presoma collected in step (2) in air atmosphere, after high-temperature calcination, naturally cool to room temperature, porous spherical lithium titanate/composite titania material can be obtained.
3. preparation method according to claim 2, it is characterized in that, in the mixed solution that step (1) obtains, in mixed solution, the molar ratio of lithium source, titanium source, surfactant, ethanol, each material of acetic acid is: 0.1-1:1:0.005-0.03:120-250:0.6-7.
4. the preparation method according to Claims 2 or 3, is characterized in that, the described lithium source of step (1) is selected from lithium nitrate, lithium chloride, lithium acetate.
5. preparation method according to claim 2, is characterized in that, described titanium source is selected from butyl titanate.
6. preparation method according to claim 2, is characterized in that, step (1) described surfactant be P123, F127, CTAB any one.
7. preparation method according to claim 2, is characterized in that, described in step (2), the power of atomizer is 35W, and frequency is 1.7MHz.
8. preparation method according to claim 2, is characterized in that, it is 450-480 DEG C that furnace temperature is decomposed in the drying of high temperature furnace described in step (2).
9. preparation method according to claim 2, is characterized in that, described in step (3), high-temperature calcination condition is: programming rate 5 DEG C/min, at 600 DEG C of calcining 4-8h.
10. an application for spherical porous lithium titanate/composite titania material according to claim 1, is characterized in that, as the application of electrode material.
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| CN105489858A (en) * | 2015-12-09 | 2016-04-13 | 南阳师范学院 | Preparation method of flower-like lithium titanate-titanium dioxide composite electrode material |
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| CN106784722A (en) * | 2017-01-11 | 2017-05-31 | 广东工业大学 | A kind of lithium titanate/titanium dioxide combination electrode material and preparation method thereof |
| CN107331841A (en) * | 2017-06-28 | 2017-11-07 | 陕西科技大学 | A kind of preparation method of lithium titanate/composite titania material |
| CN108281620A (en) * | 2017-12-15 | 2018-07-13 | 上海电力学院 | A kind of preparation method of anode material of lithium-ion battery titanium dioxide |
| CN109473656A (en) * | 2018-11-27 | 2019-03-15 | 深圳大学 | A kind of nitridation lithium titanate/nitrided silicon dioxide titanium combination electrode material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105489858A (en) * | 2015-12-09 | 2016-04-13 | 南阳师范学院 | Preparation method of flower-like lithium titanate-titanium dioxide composite electrode material |
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| CN107331841A (en) * | 2017-06-28 | 2017-11-07 | 陕西科技大学 | A kind of preparation method of lithium titanate/composite titania material |
| CN107331841B (en) * | 2017-06-28 | 2019-08-06 | 陕西科技大学 | A kind of preparation method of lithium titanate/composite titania material |
| CN108281620A (en) * | 2017-12-15 | 2018-07-13 | 上海电力学院 | A kind of preparation method of anode material of lithium-ion battery titanium dioxide |
| CN109473656A (en) * | 2018-11-27 | 2019-03-15 | 深圳大学 | A kind of nitridation lithium titanate/nitrided silicon dioxide titanium combination electrode material and preparation method thereof |
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