CN103346298A - Preparation method for lithium titanate-titanium oxide composite electrode material - Google Patents
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Abstract
The invention discloses a preparation method for a lithium titanate-titanium oxide composite electrode material. The method comprises: taking lithium hydroxide and titanium tetraisopropoxide as reaction raw materials, polyvinylpyrrolidone (PVP) as a dispersant and a diaphragm, ammonia water as a pH conditioning agent, a mixed liquor of glycol and deionized water as a solvent, carrying out a hydrothermal reaction, centrifuging, washing, drying, and heat processing to obtain the lithium titanate-titanium oxide composite material. The prepared material is high in dispersibility, fine in particle, plentiful in phase interface, high in specific charge/discharge capacity, excellent in rate capability, and the like. The method has easy technology, easy-controlling phase compositions and particle size, and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of high rate lithium ionic cell cathode lithium titanate-titanium oxide composite material, have broad application prospects in fields such as portable electric appts, power vehicle and electrical network energy storage.
Background technology
Lithium ion battery has advantages such as energy density height, output voltage height and long service life because of it, become the ideal source of portable type electronic product, also is the first-selected energy of electric automobile and hybrid vehicle.What the negative pole of current business-like lithium ion battery mainly adopted is embedding lithium material with carbon element, because electrode potential and the lithium metal of material with carbon element are very approaching, easily cause the generation of " Li dendrite ", thereby has brought bigger potential safety hazard.In addition, carbon negative pole material can form the SEI film when first charge-discharge, causes bigger irreversible capacity loss.Spinel lithium titanate is a kind of desirable lithium ion battery negative material, and its change in volume in having charge and discharge process is little, and the laudatory title of " zero strain " material is arranged; Embedding lithium current potential height (1.55V vs.Li
+/ Li), can not cause the generation of Li dendrite in the charge and discharge process, the fail safe that has improved battery; The lithium ion diffusion coefficient can fast charging and discharging than the high order of magnitude of material with carbon element.Lithium titanate possessed electrokinetic cell necessary discharge and recharge speed fast, discharge and recharge good with fail safe often characteristic.
At present, the lithium titanate problem demanding prompt solution is to improve its big high rate performance.The approach of current raising lithium titanate high rate performance mainly comprises element doping, surface modification and reduces particle size.Though above-mentioned approach can improve the chemical property of lithium titanate to a certain extent, yet because the theoretical capacity of lithium titanate only is 175mAhg
-1, make its charging and discharging capacity limited.Titanium oxide also is the good negative material of a kind of application prospect, and it has lithium ion embedding fast/take off performance.In addition, it also has electronic conductivity and the theoretical capacity (336mAhg high than spinel lithium titanate
-1).Therefore, titanium oxide is introduced in the lithium titanate material, helped to improve the charging and discharging capacity of lithium titanate.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of lithium titanate-titanium oxide composite nano-electrode material.By the mol ratio of conditioned reaction thing lithium/titanium, concentration and the hydrothermal temperature of polyvinylpyrrolidone, can regulate the relative amount of lithium titanate and titanium oxide.Lithium titanate-titanium oxide the composite material of preparation has high specific discharge capacity and excellent multiplying power cycle performance.
Technical scheme of the present invention is:
The preparation method of a kind of lithium titanate-titanium oxide combination electrode material, this preparation method is reaction raw materials with lithium hydroxide and titanium tetraisopropylate, polyvinylpyrrolidone is dispersant and barrier film, ammoniacal liquor is pH value conditioning agent, the mixed liquor of ethylene glycol and deionized water is solvent, obtain lithium titanate-titanium oxide composite material through hydro-thermal reaction, centrifugation, washing, drying and heat treatment, concrete preparation process is as follows:
(1) measure the 25mL ethylene glycol solution, utilize water-bath to be heated to 90 ℃, add a certain amount of polyvinylpyrrolidine under stirring condition, wherein the concentration of polyvinylpyrrolidine is the 0.0001-0.01 mol;
(2) titanium tetraisopropylate is joined in the above-mentioned solution, magnetic agitation 2-60 minute, obtain clear solutions; In addition, lithium hydroxide at first is dissolved in the deionized water of 5mL; Under stirring condition, slowly join in the above-mentioned settled solution then, obtain containing the solution of lithium titanium mixture; Wherein, the concentration of lithium hydroxide is the 0.001-2.5 mol, and the concentration of titanium tetraisopropylate is the 0.015-3.0 mol;
(3) be in the solution of 28% the ammoniacal liquor lithium titanium mixture that is added drop-wise to step (2) gained with mass fraction, form the milky suspension-turbid liquid, wherein the addition of ammoniacal liquor be the 1-100 milliliter/liter;
(4) the above-mentioned milky suspension-turbid liquid that obtains is transferred in the teflon-lined stainless steel cauldron, carries out hydro-thermal reaction under 100-240 ℃, the hydro-thermal time is 1-48 hour;
(5) be cooled to room temperature after the reaction, with the white precipitate centrifugation that obtains, use deionized water and absolute ethanol washing for several times respectively, then sediment was descended dry 1-24 hour at 60-120 ℃, the product with drying obtained lithium titanate-titanium oxide combination electrode material at 400-1000 ℃ of following heat treatment 1-36 hour at last.
A kind of substituting in described polyvinylpyrrolidone lauryl sodium sulfate, softex kw, the neopelex, its raw material concentration is constant.
Described lithium hydroxide substitutes with a kind of in lithium carbonate, lithium acetate, the lithium nitrate or two kinds.
A kind of substituting in described titanium tetraisopropylate butyl titanate, titanyl sulfate, the titanium tetrachloride.
When the concentration of polyvinylpyrrolidone was the 0.0001-0.008 mol described in the step (1), described lithium titanate was nano lithium titanate.
Hydrothermal temperature described in the step (4) is 100-200 ℃, and the hydro-thermal time is 2-30 hour.
Heat treatment temperature described in the step (5) is 400-800 ℃, and heat treatment time is 1-15 hour.
Exist a large amount of boundaries in the described combination electrode material, make it have pseudo-capacity effect.
The present invention has the following advantages:
1) the present invention can pass through the mol ratio of conditioned reaction thing lithium/titanium, concentration and the hydrothermal temperature of polyvinylpyrrolidone, can
To regulate the relative amount of lithium titanate and titanium oxide, obtain the good negative material of chemical property.
2) in the lithium titanate-titanium oxide composite material of the present invention's preparation, exist a large amount of boundaries, make it have pseudo-electric capacity
Effect has improved high rate performance and the specific discharge capacity of material.
3) sample dispersion of the present invention's preparation is good, and particle is tiny, has shortened the diffusion length of lithium ion.
4) technology of the present invention is simple, and thing phase constituent, particle size are easy to control, and it is compound to be widely used in other inorganic functional
The preparation of material.
Description of drawings
Fig. 1 is the X-ray diffraction analysis of the lithium titanate-titanium oxide composite material of the embodiment of the invention 1 preparation.
Fig. 2 is the field emission Electronic Speculum figure of the lithium titanate-titanium oxide composite material of the embodiment of the invention 1 preparation.
Fig. 3 is the transmission electron microscope picture of the lithium titanate-titanium oxide composite material of the embodiment of the invention 1 preparation.
Fig. 4 is the high-resolution-ration transmission electric-lens figure of the lithium titanate-titanium oxide composite material of the embodiment of the invention 1 preparation.
Fig. 5 is the cycle performance curve of the lithium titanate-titanium oxide composite material of the embodiment of the invention 1 preparation.
Embodiment
Embodiment one
(1) measure the 25mL ethylene glycol solution, utilize water-bath to be heated to 90 ℃, add a certain amount of polyvinylpyrrolidine under stirring condition, wherein the concentration of polyvinylpyrrolidine is the 0.0002-0.008 mol;
(2) titanium tetraisopropylate is joined in the above-mentioned solution, magnetic agitation 5-45 minute, obtain clear solutions; In addition, lithium hydroxide at first is dissolved in the deionized water of 5mL; Under stirring condition, slowly join in the above-mentioned settled solution then, obtain containing the solution of lithium titanium mixture; Wherein, the concentration of lithium hydroxide is the 0.05-2.0 mol, and the concentration of titanium tetraisopropylate is the 0.06-2.7 mol;
(3) be in the solution of 28% the ammoniacal liquor lithium titanium mixture that is added drop-wise to step (2) gained with mass fraction, form the milky suspension-turbid liquid, wherein the addition of ammoniacal liquor be the 5-80 milliliter/liter;
(4) the above-mentioned milky suspension-turbid liquid that obtains is transferred in the teflon-lined stainless steel cauldron, carries out hydro-thermal reaction under 100-200 ℃, the hydro-thermal time is 5-48 hour;
(5) be cooled to room temperature after the reaction, with the white precipitate centrifugation that obtains, use deionized water and absolute ethanol washing for several times respectively, then with sediment at 60-100
℃Dry 3-20 hour down, the product with drying obtained lithium titanate-titanium oxide combination electrode material at 400-850 ℃ of following heat treatment 1-26 hour at last.
Embodiment two
(1) measure the 25mL ethylene glycol solution, utilize water-bath to be heated to 90 ℃, add a certain amount of polyvinylpyrrolidine under stirring condition, wherein the concentration of polyvinylpyrrolidine is the 0.0012-0.008 mol;
(2) butyl titanate is joined in the above-mentioned solution, magnetic agitation 15-40 minute, obtain clear solutions; In addition, lithium hydroxide at first is dissolved in the deionized water of 5mL; Under stirring condition, slowly join in the above-mentioned settled solution then, obtain containing the solution of lithium titanium mixture; Wherein, the concentration of lithium hydroxide is the 0.12-1.8 mol, and the concentration of butyl titanate is the 0.13-2.3 mol;
(3) be in the solution of 28% the ammoniacal liquor lithium titanium mixture that is added drop-wise to step (2) gained with mass fraction, form the milky suspension-turbid liquid, wherein the addition of ammoniacal liquor be the 8-72 milliliter/liter;
(4) the above-mentioned milky suspension-turbid liquid that obtains is transferred in the teflon-lined stainless steel cauldron, carries out hydro-thermal reaction under 110-180 ℃, the hydro-thermal time is 6-38 hour;
(5) be cooled to room temperature after the reaction, with the white precipitate centrifugation that obtains, use deionized water and absolute ethanol washing for several times respectively, then sediment was descended dry 3-16 hour at 65-100 ℃, the product with drying obtained lithium titanate-titanium oxide combination electrode material at 470-800 ℃ of following heat treatment 3-16 hour at last.
Embodiment three
(1) measure the 25mL ethylene glycol solution, utilize water-bath to be heated to 90 ℃, add a certain amount of softex kw under stirring condition, wherein the concentration of softex kw is the 0.0011-0.008 mol;
(2) titanium tetraisopropylate is joined in the above-mentioned solution, magnetic agitation 5-35 minute, obtain clear solutions; In addition, lithium nitrate at first is dissolved in the deionized water of 5mL; Under stirring condition, slowly join in the above-mentioned settled solution then, obtain containing the solution of lithium titanium mixture; Wherein, the concentration of lithium nitrate is the 0.11-1.6 mol, and the concentration of titanium tetraisopropylate is the 0.12-2.1 mol;
(3) be in the solution of 28% the ammoniacal liquor lithium titanium mixture that is added drop-wise to step (2) gained with mass fraction, form the milky suspension-turbid liquid, wherein the addition of ammoniacal liquor be the 8-72 milliliter/liter;
(4) the above-mentioned milky suspension-turbid liquid that obtains is transferred in the teflon-lined stainless steel cauldron, carries out hydro-thermal reaction under 80-170 ℃, the hydro-thermal time is 2-30 hour;
(5) be cooled to room temperature after the reaction, with the white precipitate centrifugation that obtains, use deionized water and absolute ethanol washing for several times respectively, then sediment was descended dry 3-12 hour at 70-90 ℃, the product with drying obtained lithium titanate-titanium oxide combination electrode material at 420-750 ℃ of following heat treatment 2-18 hour at last.
Embodiment four
(1) measure the 25mL ethylene glycol solution, utilize water-bath to be heated to 90 ℃, add a certain amount of softex kw under stirring condition, wherein the concentration of softex kw is the 0.0008-0.01 mol;
(2) titanyl sulfate is joined in the above-mentioned solution, magnetic agitation 5-25 minute, obtain clear solutions; In addition, lithium nitrate at first is dissolved in the deionized water of 5mL; Under stirring condition, slowly join in the above-mentioned settled solution then, obtain containing the solution of lithium titanium mixture; Wherein, the concentration of lithium nitrate is the 0.1-1.9 mol, and the concentration of four titanyl sulfates is the 0.11-2.3 mol;
(3) be in the solution of 28% the ammoniacal liquor lithium titanium mixture that is added drop-wise to step (2) gained with mass fraction, form the milky suspension-turbid liquid, wherein the addition of ammoniacal liquor be the 15-60 milliliter/liter;
(4) the above-mentioned milky suspension-turbid liquid that obtains is transferred in the teflon-lined stainless steel cauldron, carries out hydro-thermal reaction under 120-170 ℃, the hydro-thermal time is 5-24 hour;
(5) be cooled to room temperature after the reaction, with the white precipitate centrifugation that obtains, use deionized water and absolute ethanol washing for several times respectively, then sediment was descended dry 5-11 hour at 72-85 ℃, the product with drying obtained lithium titanate-titanium oxide combination electrode material at 470-720 ℃ of following heat treatment 2-18 hour at last.
Embodiment five
(1) measure the 25mL ethylene glycol solution, utilize water-bath to be heated to 90 ℃, add a certain amount of lauryl sodium sulfate under stirring condition, wherein the concentration of lauryl sodium sulfate is the 0.0013-0.01 mol;
(2) butyl titanate is joined in the above-mentioned solution, magnetic agitation 10-35 minute, obtain clear solutions; In addition, lithium acetate at first is dissolved in the deionized water of 5mL; Under stirring condition, slowly join in the above-mentioned settled solution then, obtain containing the solution of lithium titanium mixture; Wherein, the concentration of lithium acetate is the 0.1-1.3 mol, and the concentration of butyl titanate is the 0.12-1.7 mol;
(3) be in the solution of 28% the ammoniacal liquor lithium titanium mixture that is added drop-wise to step (2) gained with mass fraction, form the milky suspension-turbid liquid, wherein the addition of ammoniacal liquor be the 20-55 milliliter/liter;
(4) the above-mentioned milky suspension-turbid liquid that obtains is transferred in the teflon-lined stainless steel cauldron, carries out hydro-thermal reaction under 100-160 ℃, the hydro-thermal time is 6-30 hour;
(5) be cooled to room temperature after the reaction, with the white precipitate centrifugation that obtains, use deionized water and absolute ethanol washing for several times respectively, then sediment was descended dry 3-15 hour at 70-90 ℃, the product with drying obtained lithium titanate-titanium oxide combination electrode material at 510-750 ℃ of following heat treatment 2-15 hour at last.
Embodiment six
(1) measure the 25mL ethylene glycol solution, utilize water-bath to be heated to 90 ℃, add a certain amount of neopelex under stirring condition, wherein the concentration of neopelex is the 0.0015-0.009 mol;
(2) titanium tetrachloride is joined in the above-mentioned solution, magnetic agitation 8-30 minute, obtain clear solutions; In addition, lithium carbonate at first is dissolved in the deionized water of 5mL; Under stirring condition, slowly join in the above-mentioned settled solution then, obtain containing the solution of lithium titanium mixture; Wherein, the concentration of lithium carbonate is the 0.08-1.2 mol, and the concentration of titanium tetrachloride is the 0.09-1.9 mol;
(3) be in the solution of 28% the ammoniacal liquor lithium titanium mixture that is added drop-wise to step (2) gained with mass fraction, form the milky suspension-turbid liquid, wherein the addition of ammoniacal liquor be the 25-50 milliliter/liter;
(4) the above-mentioned milky suspension-turbid liquid that obtains is transferred in the teflon-lined stainless steel cauldron, carries out hydro-thermal reaction under 120-170 ℃, the hydro-thermal time is 6-35 hour;
(5) be cooled to room temperature after the reaction, with the white precipitate centrifugation that obtains, use deionized water and absolute ethanol washing for several times respectively, then sediment was descended dry 2-10 hour at 65-80 ℃, the product with drying obtained lithium titanate-titanium oxide combination electrode material at 550-700 ℃ of following heat treatment 2-9 hour at last.
Claims (8)
1. the preparation method of lithium titanate-titanium oxide combination electrode material is characterized in that:
This preparation method is reaction raw materials with lithium hydroxide and titanium tetraisopropylate, polyvinylpyrrolidone is dispersant and barrier film, ammoniacal liquor is pH value conditioning agent, the mixed liquor of ethylene glycol and deionized water is solvent, obtain lithium titanate-titanium oxide composite material through hydro-thermal reaction, centrifugation, washing, drying and heat treatment, concrete preparation process is as follows:
(1) measure the 25mL ethylene glycol solution, utilize water-bath to be heated to 90 ° of C, add a certain amount of polyvinylpyrrolidine under stirring condition, wherein the concentration of polyvinylpyrrolidine is the 0.0001-0.01 mol;
(2) titanium tetraisopropylate is joined in the above-mentioned solution, magnetic agitation 2-60 minute, obtain clear solutions; In addition, lithium hydroxide at first is dissolved in the deionized water of 5mL; Under stirring condition, slowly join in the above-mentioned settled solution then, obtain containing the solution of lithium titanium mixture; Wherein, the concentration of lithium hydroxide is the 0.001-2.5 mol, and the concentration of titanium tetraisopropylate is the 0.015-3.0 mol;
(3) be in the solution of 28% the ammoniacal liquor lithium titanium mixture that is added drop-wise to step (2) gained with mass fraction, form the milky suspension-turbid liquid, wherein the addition of ammoniacal liquor be the 1-100 milliliter/liter;
(4) the above-mentioned milky suspension-turbid liquid that obtains is transferred in the teflon-lined stainless steel cauldron, carries out hydro-thermal reaction under 100-240 ° of C, the hydro-thermal time is 1-48 hour;
(5) be cooled to room temperature after the reaction, with the white precipitate centrifugation that obtains, use deionized water and absolute ethanol washing for several times respectively, then with sediment under 60-120 ° of C dry 1-24 hour, at last the product of drying was obtained lithium titanate-titanium oxide combination electrode material in heat treatment 1-36 hour under 400-1000 ° of C.
2. the preparation method of a kind of lithium titanate according to claim 1-titanium oxide combination electrode material is characterized in that:
A kind of substituting in described polyvinylpyrrolidone lauryl sodium sulfate, softex kw, the neopelex, its raw material concentration is constant.
3. the preparation method of a kind of lithium titanate according to claim 1-titanium oxide combination electrode material is characterized in that:
Described lithium hydroxide substitutes with a kind of in lithium carbonate, lithium acetate, the lithium nitrate or two kinds.
4. the preparation method of a kind of lithium titanate according to claim 1-titanium oxide combination electrode material is characterized in that:
A kind of substituting in described titanium tetraisopropylate butyl titanate, titanyl sulfate, the titanium tetrachloride.
5. according to the preparation method of each described a kind of lithium titanate-titanium oxide combination electrode material of claim 1 to 4, it is characterized in that:
When the concentration of polyvinylpyrrolidone was the 0.0001-0.008 mol described in the step (1), described lithium titanate was nano lithium titanate.
6. according to the preparation method of each described a kind of lithium titanate-titanium oxide combination electrode material of claim 1 to 4, it is characterized in that:
Hydrothermal temperature described in the step (4) is 100-200 ° of C, and the hydro-thermal time is 2-30 hour.
7. according to the preparation method of each described a kind of lithium titanate-titanium oxide combination electrode material of claim 1 to 4, it is characterized in that: the heat treatment temperature described in the step (5) is 400-800 ° of C, and heat treatment time is 1-15 hour.
8. the preparation method of a kind of lithium titanate according to claim 1-titanium oxide combination electrode material is characterized in that: exist a large amount of boundaries in the described combination electrode material, make it have pseudo-capacity effect.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104409694A (en) * | 2014-11-18 | 2015-03-11 | 南阳师范学院 | Preparation method of globular-flower-shaped Li4Ti5O12-TiO2 composite electrode material |
| CN109336169A (en) * | 2018-09-29 | 2019-02-15 | 南京大学射阳高新技术研究院 | A kind of controllable synthesis method of lithium titanate micron-size spherical secondary structure and its application |
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| CN102107906A (en) * | 2010-12-30 | 2011-06-29 | 清华大学深圳研究生院 | Method for preparing lithium titanate material |
| CN102386385A (en) * | 2011-10-09 | 2012-03-21 | 北京科技大学 | Preparation method of Li4Ti5O12-TiO2 composite electrode material |
| CN102956880A (en) * | 2012-11-15 | 2013-03-06 | 华中科技大学 | Method for preparing Li4Ti5O12-TiO2 (lithium titanate - titanium oxide) nano composite material and Li4Ti5O12-TiO2 nano composite material thereof |
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| US20010031401A1 (en) * | 1999-02-16 | 2001-10-18 | Tetsuya Yamawaki | Process for producing lithium titanate and lithium ion battery and negative electrode therein |
| CN102107906A (en) * | 2010-12-30 | 2011-06-29 | 清华大学深圳研究生院 | Method for preparing lithium titanate material |
| CN102386385A (en) * | 2011-10-09 | 2012-03-21 | 北京科技大学 | Preparation method of Li4Ti5O12-TiO2 composite electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104409694A (en) * | 2014-11-18 | 2015-03-11 | 南阳师范学院 | Preparation method of globular-flower-shaped Li4Ti5O12-TiO2 composite electrode material |
| CN109336169A (en) * | 2018-09-29 | 2019-02-15 | 南京大学射阳高新技术研究院 | A kind of controllable synthesis method of lithium titanate micron-size spherical secondary structure and its application |
| CN109336169B (en) * | 2018-09-29 | 2020-10-09 | 南京大学射阳高新技术研究院 | Controllable synthesis method and application of lithium titanate micron-sized spherical secondary structure |
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