CN104009236B - A kind of metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material and its preparation method and application - Google Patents
A kind of metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material and its preparation method and application Download PDFInfo
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- CN104009236B CN104009236B CN201410256213.0A CN201410256213A CN104009236B CN 104009236 B CN104009236 B CN 104009236B CN 201410256213 A CN201410256213 A CN 201410256213A CN 104009236 B CN104009236 B CN 104009236B
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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Abstract
The present invention discloses a kind of metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material and its preparation method and application, and described mesoporous single crystals nano-particle diameter is 30��60nm, and Jie hole pore size distribution is 2��8nm. Preparation method is as follows: mixing after being dispersed in alcohol solvent respectively by titanium source and graphene oxide, then a little deionized water and the mixing solutions of ethanol is added, at 100 DEG C, backflow is prepared into titanium dioxide/graphene oxide matrix material, then hydrothermal method redox graphene is utilized, again itself and lithium source are carried out hydro-thermal lithiation, finally heat-treat under an argon atmosphere, metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material can be obtained. Prepared metatitanic acid lithium mesoporous single crystals nano particle has abundant electrochemical site, the introducing of redox graphene is conducive to improving the electronic conductivity of metatitanic acid lithium, electro-chemical test shows good performance, is expected to obtain in field of lithium ion battery apply widely.
Description
Technical field
The invention belongs to new energy materials field, it relates to a kind of lithium ion battery cathode material and its preparation method and application, specifically, described lithium ion battery negative material relates to a kind of metatitanic acid lithium (Li with mesoporous single crystals shape looks4Ti5O12)/redox graphene matrix material.
Background technology
Lithium ion battery has the advantage such as bigger energy density and longer cycle life because of it so that it is occupy more and more important status in the field such as portable electric appts, electromobile. But the development along with science and technology, lithium ion battery be it is also proposed higher requirement by people. Electrode materials is one of key issue of lithium ion battery needs solution. Current commercial li-ion cell negative electrode material mainly carbon material, but the lower (0.2Vvs.Li/Li of the operating potential of carbon material+), when overcharge, carbon material surface easily forms Li dendrite thus causes safety problem. Find safer, high rate performance and the better negative material of cycle performance, become the focus of Study on Li-ion batteries.
In recent years, spinel Li4Ti5O12Day by day paid attention to as new negative electrode materials for lithium secondary batteries. As " zero strain " material, there is superior cyclical stability; And it has higher intercalation potential (1.55Vvs.Li/Li+) and not easily cause metallic lithium to precipitate out, security is good. But pure phase Li4Ti5O12Electroconductibility is not good, causes high rate performance undesirable, becomes and limits one of its main bottleneck developed. At present for Li4Ti5O12The method carrying out improving mainly contain composition optimizes and with carbon material compound etc. Such as, the people such as Yu (L.Yu, H.B.WuandX.W.D.Lou, AdvancedMaterials, 2013,25,2296-2300.) do Template preparation with silicon ball and have gone out Jie hole Li4Ti5O12Hollow spheres, still keeps 104mAhg under the charge-discharge magnification of 20C-1Capacity.The people such as Shen (L.Shen, X.Zhang, E.Uchaker, C.YuanandG.Cao, AdvancedEnergyMaterials, 2012,2,691-698.) are by Li4Ti5O12Load obtains matrix material on ordered mesopore carbon, and the charge/discharge capacity at 40C can reach 92.6mAhg-1, with the high rate performance of material after ordered mesopore carbon compound be improved significantly.
Summary of the invention
In view of above problem, it is an object of the invention to provide a kind of metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material and its preparation method and application, mentality of designing is as follows:
Prepare TiO with hydrolysis method2Nano particle/graphene oxide matrix material, then hydrothermal method redox graphene is utilized, again itself and lithium source are carried out hydro-thermal lithiation, heat-treat under an argon atmosphere after cleaning, prepare metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material. In prepared matrix material, Li4Ti5O12The mesoporous single crystals structure of nano particle can significantly increase its electrochemical site, and the introducing of redox graphene not only contributes to improving Li4Ti5O12The electroconductibility of nano particle, it is also possible to prevent the reunion of nano particle in lithiumation process, ensure that the electrochemical activity that matrix material is high and high rate capability.
The concrete technical scheme of the present invention is as follows:
A kind of metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material, described matrix material has following structure: metatitanic acid lithium mesoporous single crystals nano particle load is on redox graphene; Wherein, the diameter of metatitanic acid lithium mesoporous single crystals nano particle is 30��60nm, and Jie hole pore size distribution is 2��8nm, and weight percentage is 70��95%.
A preparation method for metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material, comprises the steps:
(1) graphene oxide is prepared;
(2) graphene oxide that 30��100mg step (1) obtains is dispersed in 200��500ml ethanol, ultrasonic disperse 2��5h, obtain dispersion liquid, it is added drop-wise in described dispersion liquid after 1��3g tetrabutyl titanate is mixed with the ethanol of homogenous quantities, stir 20��60min, obtain mixing solutions;
(3) being mixed with the ethanol of homogenous quantities by 1��3g deionized water, add the mixing solutions described in step (2), stir 20��60min, reflux 5��20h at 100 DEG C, is cooled to room temperature, takes out filter, repeatedly cleans with ethanol and collect product;
(4) product of step (3) is dispersed in 100��200ml deionized water, at 120��200 DEG C of hydrothermal reduction 4��20h, after centrifuge washing lyophilize, collects product;
(5), after being mixed with the lithium hydroxide solution of 0.4��1.2mol/L by the product of step (4), 160��200 DEG C of hydro-thermal lithiation 8��16h, collect product after centrifuge washing drying;
(6) by the product of step (5) in argon gas atmosphere at 400��700 DEG C thermal treatment 2��6h, described metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material can be obtained. The structure of described matrix material is: metatitanic acid lithium mesoporous single crystals nano particle load is on redox graphene; Wherein, the diameter of metatitanic acid lithium mesoporous single crystals nano particle is 30��60nm, and Jie hole pore size distribution is 2��8nm, and in matrix material, the weight percentage of metatitanic acid lithium mesoporous single crystals nano particle is 70��95%.
Described step (1) is specially: natural flake graphite and SODIUMNITRATE are mixed, add the vitriol oil, ice-water bath stirs 10��20min, slowly add potassium permanganate again, ice-water bath reacts 0.5��1h, continuously stirring 72��120h at 20��25 DEG C, adds deionized water and the hydrogen peroxide reaction 2��3h of 50��60 DEG C, centrifugation successively;Separated product is successively with the mixing solutions of sulfuric acid and hydrogen peroxide, hydrochloric acid dilute solution and deionized water wash 3 times, then centrifuge washing is to neutral; Adding 20��50mL deionized water ultrasonic disperse 3��5h, lyophilize obtains graphene oxide.
The mass ratio of the deionized water in described step (3) and the tetrabutyl titanate in step (2) is 0.5��2.
The mol ratio of lithium hydroxide and tetrabutyl titanate is 2��10.
The application of above-mentioned metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material, is applied to lithium ion battery as negative material.
By above technical scheme and implementation method it will be seen that the Li for preparing of the present invention4Ti5O12Li in/redox graphene matrix material4Ti5O12The mesoporous single crystals structure of nano particle can significantly increase its electrochemical site, it is to increase its electrochemical activity, and the introducing of redox graphene not only contributes to improving Li4Ti5O12The electroconductibility of nano particle, it is also possible to prevent the reunion of nano particle in lithiumation process, ensure that the electrochemical activity that matrix material is high and high rate capability, is applied in lithium ion battery negative material field and has excellent high rate performance and cyclical stability.
Accompanying drawing explanation
Fig. 1 is the XRD curve of embodiment 1 product;
Fig. 2 is the transmission electron microscope photo of embodiment 1 product;
Fig. 3 is the Electrochemical results of product as lithium ion battery negative material of embodiment 1.
Embodiment
Below in conjunction with drawings and Examples, specific embodiments of the present invention are further described in detail, but should not limit the scope of the invention with this.
Embodiment 1
Prepare graphene oxide: 1g natural flake graphite and 1g SODIUMNITRATE are mixed, add the 60mL vitriol oil, ice-water bath stirs 10��20min, slowly add 6g potassium permanganate again, ice-water bath reacts 0.5h, continuously stirring 120h at 25 DEG C, add deionized water and the 15mL hydrogen peroxide of 60ml50��60 DEG C successively, respectively react 2h, centrifugation; Separated product is successively with the mixing solutions of sulfuric acid and hydrogen peroxide, hydrochloric acid dilute solution and deionized water wash 3 times, then centrifuge washing is to neutral; Adding 20mL deionized water ultrasonic disperse 5h, lyophilize obtains graphene oxide.
Being dispersed in 300ml ethanol by the graphene oxide of 60mg, ultrasonic disperse 3h, obtains dispersion liquid, is mixed with 2g ethanol by 2g tetrabutyl titanate, is added drop-wise in dispersion liquid, stirs 30min, obtains mixing solutions;
Being mixed with 2g ethanol by 2g deionized water, add in above-mentioned mixing solutions, stir 30min, reflux at 100 DEG C 6h, is cooled to room temperature, takes out filter, repeatedly cleans with ethanol and collects product; Being dispersed in by product in 150ml deionized water, 180 DEG C of hydrothermal reduction 6h, are cooled to room temperature, and product postlyophilization is collected in washing;
The lithium hydroxide solution that the product obtained after drying and 30ml concentration are 0.8mol/L is mixed, hydro-thermal lithiumation 10h at 180 DEG C; By dry for products therefrom washing after cooling, 600 DEG C of thermal treatment 2h under an argon atmosphere, have the Li of mesoporous single crystals shape looks described in can obtaining4Ti5O12/ redox graphene matrix material.
The XRD curve of product as shown in Figure 1, the transmission electron microscope photo of product as shown in Figure 2. Wherein, Li4Ti5O12For mesoporous single crystals nano particle, its diameter is 30��60nm, and Jie hole pore size distribution is 2��8nm.
Used as lithium ion battery negative material, CR2016 type button cell is adopted to test its chemical property. Fig. 3 is the multiplying power discharging test result figure of material, and as can be seen from Figure 3 along with the increase of current density, the decline of its capacity is relatively slower, illustrates that this kind of material has good high rate performance.And the circulation volume under same current density keeps stable, when current density returns low range, capacity can well recover, and proves that this kind of material has good cyclical stability.
Embodiment 2
Prepare graphene oxide: repeat example 1. Being dispersed in 450ml ethanol by the graphene oxide of 90mg, ultrasonic disperse 5h, obtains dispersion liquid, is mixed with 3g ethanol by 3g tetrabutyl titanate, is added drop-wise in dispersion liquid, stirs 30min, obtains mixing solutions;
Being mixed with 3g ethanol by 3g deionized water, add in above-mentioned mixing solutions, stir 60min, reflux at 110 DEG C 10h, is cooled to room temperature, takes out filter, repeatedly cleans with ethanol and collects product; Being dispersed in by product in 200ml deionized water, 160 DEG C of hydrothermal reduction 10h, are cooled to room temperature, wash and collect product, lyophilize;
The lithium hydroxide solution that the product obtained after drying and 45ml concentration are 0.7mol/L is mixed, hydro-thermal lithiumation 10h at 180 DEG C; By dry for products therefrom washing after cooling, the lower 500 DEG C of thermal treatment 3h of argon gas atmosphere, can obtain the Li of mesoporous single crystals shape looks4Ti5O12/ redox graphene matrix material. Electro-chemical test part illustrates the experimental result almost identical with embodiment 1 with embodiment 1, prepared material.
Embodiment 3
Prepare graphene oxide: repeat example 1. Being dispersed in 150ml ethanol by the graphene oxide of 30mg, ultrasonic disperse 5h, obtains dispersion liquid, is mixed with 1g ethanol by 1g titanium isopropylate, is added drop-wise in dispersion liquid, stirs 30min, obtains mixing solutions;
Being mixed with 1g ethanol by 1g deionized water, add in above-mentioned mixing solutions, stir 30min, reflux at 90 DEG C 8h, is cooled to room temperature, takes out filter, repeatedly cleans with ethanol and collects product; Being dispersed in by product in 100ml deionized water, 200 DEG C of hydrothermal reduction 5h, are cooled to room temperature, collect product lyophilize after washing;
The lithium hydroxide solution that the product obtained after drying and 20ml concentration are 0.8mol/L is mixed, hydro-thermal lithiumation 10h at 180 DEG C; By dry for products therefrom washing after cooling, the lower 700 DEG C of thermal treatment 5h of argon gas atmosphere, can obtain mesoporous single crystals shape looks Li4Ti5O12/ redox graphene matrix material. Electro-chemical test part illustrates the experimental result almost identical with embodiment 1 with embodiment 1, prepared material.
Claims (6)
1. metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material, it is characterised in that, described matrix material has following structure: metatitanic acid lithium mesoporous single crystals nano particle load is on redox graphene; Wherein, the diameter of metatitanic acid lithium mesoporous single crystals nano particle is 30��60nm, and Jie hole pore size distribution is 2��8nm, and weight percentage is 70��95%; The preparation method of described matrix material comprises the steps:
(1) graphene oxide is prepared;
(2) graphene oxide that 30��100mg step (1) obtains is dispersed in 200��500ml ethanol, ultrasonic disperse 2��5h, obtain dispersion liquid, it is added drop-wise in described dispersion liquid after 1��3g tetrabutyl titanate is mixed with the ethanol of homogenous quantities, stir 20��60min, obtain mixing solutions;
(3) being mixed with the ethanol of homogenous quantities by 1��3g deionized water, add the mixing solutions described in step (2), stir 20��60min, reflux 5��20h at 100 DEG C, is cooled to room temperature, takes out filter, repeatedly cleans with ethanol and collect product;
(4) product of step (3) is dispersed in 100��200ml deionized water, at 120��200 DEG C of hydrothermal reduction 4��20h, after centrifuge washing lyophilize, collects product;
(5), after being mixed with the lithium hydroxide solution of 0.4��1.2mol/L by the product of step (4), 160��200 DEG C of hydro-thermal lithiation 8��16h, collect product after centrifuge washing drying;
(6) by the product of step (5) in argon gas atmosphere at 400��700 DEG C thermal treatment 2��6h, described metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material can be obtained.
2. matrix material according to claim 1, it is characterised in that, the structure of described matrix material is: metatitanic acid lithium mesoporous single crystals nano particle load is on redox graphene; Wherein, the diameter of metatitanic acid lithium mesoporous single crystals nano particle is 30��60nm, and Jie hole pore size distribution is 2��8nm, and in matrix material, the weight percentage of metatitanic acid lithium mesoporous single crystals nano particle is 70��95%.
3. matrix material according to claim 1, it is characterized in that, described step (1) is specially: natural flake graphite and SODIUMNITRATE are mixed, add the vitriol oil, ice-water bath stirs 10��20min, more slowly adds potassium permanganate, ice-water bath reacts 0.5��1h, continuously stirring 72��120h at 20��25 DEG C, adds deionized water and the hydrogen peroxide reaction 2��3h of 50��60 DEG C, centrifugation successively; Separated product is successively with the mixing solutions of sulfuric acid and hydrogen peroxide, hydrochloric acid dilute solution and deionized water wash 3 times, then centrifuge washing is to neutral; Adding 20��50ml deionized water ultrasonic disperse 3��5h, lyophilize obtains graphene oxide.
4. matrix material according to claim 1, it is characterised in that, the mass ratio of the deionized water in described step (3) and the tetrabutyl titanate in step (2) is 0.5��2.
5. matrix material according to claim 1, it is characterised in that, the mol ratio of lithium hydroxide and tetrabutyl titanate is 2��10.
6. the application of metatitanic acid lithium mesoporous single crystals nano particle/redox graphene matrix material according to claim 1, it is characterised in that, described matrix material is applied to lithium ion battery as negative material.
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| CN104466115A (en) * | 2014-11-19 | 2015-03-25 | 南京航空航天大学 | Preparation method and application of flexible lithium titanate-carbon composite electrode material |
| CN105206810B (en) * | 2015-09-16 | 2016-12-07 | 宁波中车新能源科技有限公司 | Nano lithium titanate composite and preparation method thereof |
| CN105336940B (en) * | 2015-10-20 | 2018-06-05 | 深圳先进技术研究院 | A kind of sodium titanate nano wire/graphene composite negative pole material and preparation method thereof |
| CN105845901B (en) * | 2016-03-28 | 2018-09-21 | 辽宁大学 | A kind of lithium ion battery negative material Li4Ti5O12/TiO2/ RGO and preparation method thereof |
| CN105720268B (en) * | 2016-04-08 | 2018-08-14 | 辽宁大学 | A kind of lithium ion battery negative material and preparation method thereof |
| CN107706362A (en) * | 2017-08-17 | 2018-02-16 | 中国第汽车股份有限公司 | A kind of preparation method of graphene combination electrode material |
| CN108134072B (en) * | 2018-01-30 | 2022-01-28 | 中国科学院宁波材料技术与工程研究所 | Lithium titanate-based composite material and preparation method thereof |
| CN108766784A (en) * | 2018-06-25 | 2018-11-06 | 南京工业大学 | A kind of self-supporting lithium titanate/grapheme foam composite anode materials and application |
| CN108529603A (en) * | 2018-06-26 | 2018-09-14 | 西南交通大学 | Alcohol heat-treats the method and graphene of graphene oxide |
| CN111312997B (en) * | 2019-03-13 | 2021-07-13 | 北京纳米能源与***研究所 | Composite material and preparation method and application thereof |
| CN110350170A (en) * | 2019-06-28 | 2019-10-18 | 陕西科技大学 | A kind of preparation method of lithium titanate/graphene composite material |
| CN113394382B (en) * | 2021-06-11 | 2022-11-15 | 北京化工大学 | Potassium titanium phosphate @ carbon-reduced graphene oxide material, preparation method thereof and potassium ion battery |
| CN113964315A (en) * | 2021-10-14 | 2022-01-21 | 北京师范大学 | Preparation method and application of large-size two-dimensional lithium titanate nanosheet |
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