CN104009236A - Lithium titanate mesoporous single-crystal nanoparticle/reduced graphene oxide composite material as well as preparation method and application thereof - Google Patents

Lithium titanate mesoporous single-crystal nanoparticle/reduced graphene oxide composite material as well as preparation method and application thereof Download PDF

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CN104009236A
CN104009236A CN201410256213.0A CN201410256213A CN104009236A CN 104009236 A CN104009236 A CN 104009236A CN 201410256213 A CN201410256213 A CN 201410256213A CN 104009236 A CN104009236 A CN 104009236A
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composite material
lithium titanate
graphene oxide
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CN104009236B (en
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江浩
李春忠
陈维纳
丁红梅
邓宗南
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East China University of Science and Technology
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • 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
    • 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
    • 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
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Abstract

The invention discloses a lithium titanate mesoporous single-crystal nanoparticle/reduced graphene oxide composite material as well as a preparation method and an application thereof. Each mesoporous single-crystal nanoparticle is between 30nm and 60nm in diameter; pore diameter of each mesoporous is within 2nm to 8nm. The preparation method comprises the following steps: respectively dispersing a titanium source and a graphene oxide in an ethyl alcohol solvent and then mixing, adding a small amount of mixed solution of deionized water and ethyl alcohol and refluxing at 100 DEG C so as to prepare a titanium dioxide/graphene oxide composite material; reducing the graphene oxide via a hydrothermal method; carrying out a hydrothermal lithiation reaction on the reduced graphene oxide and the titanium source; and finally, carrying out heat treatment under an argon atmosphere, thereby obtaining the lithium titanate mesoporous single-crystal nanoparticle/reduced graphene oxide composite material. The prepared lithium titanate mesoporous single-crystal nanoparticle is rich in electrochemical active sites; the electronic conductivity of the lithium titanate is improved via the introduction of the reduced graphene oxide, so that the prepared lithium titanate mesoporous single-crystal nanoparticle/reduced graphene oxide composite material has good performance in electrochemical testing and can be widely applied to the field of lithium ion batteries.

Description

A kind of lithium titanate mesoporous single crystals nano particle/redox graphene composite material and its preparation method and application
Technical field
The invention belongs to new energy materials field, relate to a kind of lithium ion battery cathode material and its preparation method and application, particularly, described lithium ion battery negative material relates to a kind of lithium titanate (Li with mesoporous single crystals pattern 4ti 5o 12)/redox graphene composite material.
Background technology
Lithium ion battery is because it has the advantages such as larger energy density and longer cycle life, make its in the field such as portable electric appts, electric automobile in occupation of consequence more and more.But along with scientific and technological development, people also have higher requirement to lithium ion battery.Electrode material is one of lithium ion battery key issue that need to solve.Commercial li-ion cell negative electrode material is mainly material with carbon element at present, but lower (the 0.2V vs.Li/Li of the operating potential of material with carbon element +), in the situation that overcharging, thereby easily forming Li dendrite, carbon material surface 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 using.
In recent years, spinelle Li 4ti 5o 12day by day come into one's own as new negative electrode materials for lithium secondary batteries.As " zero strain " material, there is superior cyclical stability; And it has higher embedding lithium current potential (1.55V vs.Li/Li +) and be difficult for causing that lithium metal separates out, fail safe is good.But pure phase Li 4ti 5o 12conductivity is not good, causes high rate performance undesirable, becomes one of Main Bottleneck limiting its development.At present for Li 4ti 5o 12carry out improved method and mainly contain structure optimization and compound etc. with material with carbon element.For example, the people such as Yu (L.Yu, H.B.Wu and X.W.D.Lou, Advanced Materials, 2013,25,2296-2300.) do template with silicon ball and have prepared mesoporous Li 4ti 5o 12hollow spheres still keeps 104mAh g under the charge-discharge magnification of 20C -1capacity.The people such as Shen (L.Shen, X.Zhang, E.Uchaker, C.Yuan and G.Cao, Advanced Energy Materials, 2012,2,691-698.) are by Li 4ti 5o 12load on ordered mesopore carbon and obtain composite material, can reach 92.6mAh g at the charge/discharge capacity of 40C -1, with the high rate performance of the compound rear material of ordered mesopore carbon be improved significantly.
Summary of the invention
In view of above problem, the object of this invention is to provide a kind of lithium titanate mesoporous single crystals nano particle/redox graphene composite material and its preparation method and application, mentality of designing is as follows:
Prepare TiO with Hydrolyze method 2nano particle/graphene oxide composite material, then utilize hydro thermal method redox graphene, again itself and lithium source are carried out to hydro-thermal lithiation, after cleaning, under argon gas atmosphere, heat-treat, prepare lithium titanate mesoporous single crystals nano particle/redox graphene composite material.In prepared composite material, Li 4ti 5o 12the mesoporous single crystals structure of nano particle can significantly increase its electrochemical site, and the introducing of redox graphene not only contributes to improve Li 4ti 5o 12the conductivity of nano particle, can also prevent the reunion of nano particle in lithiumation process, has ensured electro-chemical activity and high rate capability that composite material is high.
Concrete technical scheme of the present invention is as follows:
A kind of lithium titanate mesoporous single crystals nano particle/redox graphene composite material, described composite material has following structure: lithium titanate mesoporous single crystals nano particle loads on redox graphene; Wherein, the diameter of lithium titanate mesoporous single crystals nano particle is 30～60nm, and mesoporous pore-size distribution is 2～8nm, and weight percentage is 70～95%.
A preparation method for lithium titanate mesoporous single crystals nano particle/redox graphene composite material, comprises the steps:
(1) prepare graphene oxide;
(2) graphene oxide 30～100mg step (1) being obtained is dispersed in 200～500ml ethanol, ultrasonic dispersion 2～5h, obtain dispersion liquid, after being mixed with the ethanol of homogenous quantities, 1～3g butyl titanate is added drop-wise in described dispersion liquid, stir 20～60min, obtain mixed solution;
(3) 1～3g deionized water is mixed with the ethanol of homogenous quantities, add the described mixed solution of step (2), stir 20～60min, the 5～20h that refluxes at 100 DEG C, is cooled to room temperature, and suction filtration repeatedly cleans and collect product with ethanol;
(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 freeze drying, collects product;
(5), after the product of step (4) is mixed with the lithium hydroxide solution of 0.4～1.2mol/L, 160～200 DEG C of hydro-thermal lithiation 8～16h, collect product after centrifuge washing is dry;
(6) by the product of step (5) in argon gas atmosphere at 400～700 DEG C heat treatment 2～6h, can obtain described lithium titanate mesoporous single crystals nano particle/redox graphene composite material.The structure of described composite material is: lithium titanate mesoporous single crystals nano particle loads on redox graphene; Wherein, the diameter of lithium titanate mesoporous single crystals nano particle is 30～60nm, and mesoporous pore-size distribution is 2～8nm, and in composite material, the weight percentage of lithium titanate mesoporous single crystals nano particle is 70～95%.
Described step (1) is specially: natural flake graphite and sodium nitrate are mixed, add the concentrated sulfuric acid, in ice-water bath, stir 10～20min, slowly add again potassium permanganate, in ice-water bath, react 0.5～1h, continuous stirring 72～120h at 20～25 DEG C, adds deionized water and the hydrogen peroxide of 50～60 DEG C to react 2～3h, centrifugation successively; Separated product washs 3 times with mixed solution, hydrochloric acid weak solution and the deionized water of sulfuric acid and hydrogen peroxide successively, then centrifuge washing is to neutral; Add the ultrasonic dispersion 3～5h of 20～50mL deionized water, freeze drying obtains graphene oxide.
The mass ratio of the butyl titanate in the deionized water in described step (3) and step (2) is 0.5～2.
The mol ratio of lithium hydroxide and butyl titanate is 2～10.
The application of above-mentioned lithium titanate mesoporous single crystals nano particle/redox graphene composite material, is applied to lithium ion battery as negative material.
From above technical scheme and implementation method, Li prepared by the present invention 4ti 5o 12li in/redox graphene composite material 4ti 5o 12the mesoporous single crystals structure of nano particle can significantly increase its electrochemical site, improve its electro-chemical activity, and the introducing of redox graphene not only contributes to improve Li 4ti 5o 12the conductivity of nano particle, can also prevent the reunion of nano particle in lithiumation process, has ensured electro-chemical activity and high rate capability that composite material is high, is applied in lithium ion battery negative material field and has excellent high rate performance and cyclical stability.
Brief description of the drawings
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 that the product of embodiment 1 is as the Electrochemical results of lithium ion battery negative material.
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 sodium nitrate are mixed, add the 60mL concentrated sulfuric acid, in ice-water bath, stir 10～20min, slowly add again 6g potassium permanganate, in ice-water bath, react 0.5h, continuous stirring 120h at 25 DEG C, adds deionized water and the 15mL hydrogen peroxide of 60ml50～60 DEG C successively, each reaction 2h, centrifugation; Separated product washs 3 times with mixed solution, hydrochloric acid weak solution and the deionized water of sulfuric acid and hydrogen peroxide successively, then centrifuge washing is to neutral; Add the ultrasonic dispersion of 20mL deionized water 5h, freeze drying obtains graphene oxide.
The graphene oxide of 60mg is dispersed in 300ml ethanol, and ultrasonic dispersion 3h, obtains dispersion liquid, and 2g butyl titanate is mixed with 2g ethanol, is added drop-wise in dispersion liquid, stirs 30min, obtains mixed solution;
2g deionized water is mixed with 2g ethanol, add in above-mentioned mixed solution, stir 30min, the 6h that refluxes at 100 DEG C, is cooled to room temperature, and suction filtration repeatedly cleans and collect product with ethanol; Product is dispersed in 150ml deionized water, and 180 DEG C of hydrothermal reduction 6h, are cooled to room temperature, and product postlyophilization is collected in washing;
The lithium hydroxide solution that is 0.8mol/L with 30ml concentration by the product obtaining after dry mixes, hydro-thermal lithiumation 10h at 180 DEG C; After cooling, products therefrom washing is dry, 600 DEG C of heat treatment 2h under argon gas atmosphere, have the Li of mesoporous single crystals pattern described in can obtaining 4ti 5o 12/ redox graphene composite material.
The XRD curve of product as shown in Figure 1, the transmission electron microscope photo of product as shown in Figure 2.Wherein, Li 4ti 5o 12for mesoporous single crystals nano particle, its diameter is 30～60nm, and mesoporous pore-size distribution is 2～8nm.
Used as lithium ion battery negative material, adopt CR2016 type button cell 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, its capacity loss is slower, illustrates that this material has good high rate performance.And circulation volume under same current density keeps stable, in the time that current density is returned to low range, capacity can well recover, and proves that this material has good cyclical stability.
Embodiment 2
Prepare graphene oxide: repeat example 1.The graphene oxide of 90mg is dispersed in 450ml ethanol, and ultrasonic dispersion 5h, obtains dispersion liquid, and 3g butyl titanate is mixed with 3g ethanol, is added drop-wise in dispersion liquid, stirs 30min, obtains mixed solution;
3g deionized water is mixed with 3g ethanol, add in above-mentioned mixed solution, stir 60min, the 10h that refluxes at 110 DEG C, is cooled to room temperature, and suction filtration repeatedly cleans and collect product with ethanol; Product is dispersed in 200ml deionized water, and 160 DEG C of hydrothermal reduction 10h, are cooled to room temperature, wash and collect product, freeze drying;
The lithium hydroxide solution that is 0.7mol/L with 45ml concentration by the product obtaining after dry mixes, hydro-thermal lithiumation 10h at 180 DEG C; After cooling, products therefrom washing is dry, the lower 500 DEG C of heat treatment 3h of argon gas atmosphere, can obtain the Li of mesoporous single crystals pattern 4ti 5o 12/ redox graphene composite material.Electro-chemical test part is with embodiment 1, prepared materials show the experimental result almost identical with embodiment 1.
Embodiment 3
Prepare graphene oxide: repeat example 1.The graphene oxide of 30mg is dispersed in 150ml ethanol, and ultrasonic dispersion 5h, obtains dispersion liquid, and 1g tetraisopropyl titanate is mixed with 1g ethanol, is added drop-wise in dispersion liquid, stirs 30min, obtains mixed solution;
1g deionized water is mixed with 1g ethanol, add in above-mentioned mixed solution, stir 30min, the 8h that refluxes at 90 DEG C, is cooled to room temperature, and suction filtration repeatedly cleans and collect product with ethanol; Product is dispersed in 100ml deionized water, and 200 DEG C of hydrothermal reduction 5h, are cooled to room temperature, collect product freeze drying after washing;
The lithium hydroxide solution that is 0.8mol/L with 20ml concentration by the product obtaining after dry mixes, hydro-thermal lithiumation 10h at 180 DEG C; After cooling, by dry products therefrom washing, the lower 700 DEG C of heat treatment 5h of argon gas atmosphere, can obtain mesoporous single crystals pattern Li 4ti 5o 12/ redox graphene composite material.Electro-chemical test part is with embodiment 1, prepared materials show the experimental result almost identical with embodiment 1.

Claims (7)

1. lithium titanate mesoporous single crystals nano particle/redox graphene composite material, is characterized in that, described composite material has following structure: lithium titanate mesoporous single crystals nano particle loads on redox graphene; Wherein, the diameter of lithium titanate mesoporous single crystals nano particle is 30～60nm, and mesoporous pore-size distribution is 2～8nm, and weight percentage is 70～95%.
2. a preparation method for lithium titanate mesoporous single crystals nano particle/redox graphene composite material, is characterized in that, comprises the steps:
(1) prepare graphene oxide;
(2) graphene oxide 30～100mg step (1) being obtained is dispersed in 200～500ml ethanol, ultrasonic dispersion 2～5h, obtain dispersion liquid, after being mixed with the ethanol of homogenous quantities, 1～3g butyl titanate is added drop-wise in described dispersion liquid, stir 20～60min, obtain mixed solution;
(3) 1～3g deionized water is mixed with the ethanol of homogenous quantities, add the described mixed solution of step (2), stir 20～60min, the 5～20h that refluxes at 100 DEG C, is cooled to room temperature, and suction filtration repeatedly cleans and collect product with ethanol;
(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 freeze drying, collects product;
(5), after the product of step (4) is mixed with the lithium hydroxide solution of 0.4～1.2mol/L, 160～200 DEG C of hydro-thermal lithiation 8～16h, collect product after centrifuge washing is dry;
(6) by the product of step (5) in argon gas atmosphere at 400～700 DEG C heat treatment 2～6h, can obtain described lithium titanate mesoporous single crystals nano particle/redox graphene composite material.
3. preparation method according to claim 2, is characterized in that, the structure of described composite material is: lithium titanate mesoporous single crystals nano particle loads on redox graphene; Wherein, the diameter of lithium titanate mesoporous single crystals nano particle is 30～60nm, and mesoporous pore-size distribution is 2～8nm, and in composite material, the weight percentage of lithium titanate mesoporous single crystals nano particle is 70～95%.
4. preparation method according to claim 2, it is characterized in that, described step (1) is specially: natural flake graphite and sodium nitrate are mixed, add the concentrated sulfuric acid, in ice-water bath, stir 10～20min, more slowly add potassium permanganate, in ice-water bath, react 0.5～1h, continuous stirring 72～120h at 20～25 DEG C, adds deionized water and the hydrogen peroxide of 50～60 DEG C to react 2～3h, centrifugation successively; Separated product washs 3 times with mixed solution, hydrochloric acid weak solution and the deionized water of sulfuric acid and hydrogen peroxide successively, then centrifuge washing is to neutral; Add the ultrasonic dispersion 3～5h of 20～50ml deionized water, freeze drying obtains graphene oxide.
5. preparation method according to claim 2, is characterized in that, the mass ratio of the butyl titanate in the deionized water in described step (3) and step (2) is 0.5～2.
6. preparation method according to claim 2, is characterized in that, the mol ratio of lithium hydroxide and butyl titanate is 2～10.
7. the application of lithium titanate mesoporous single crystals nano particle/redox graphene composite material claimed in claim 1, is characterized in that, described combination electrode 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
CN105206810A (en) * 2015-09-16 2015-12-30 宁波南车新能源科技有限公司 Nanometer lithium titanate composite and preparation method thereof
CN105336940A (en) * 2015-10-20 2016-02-17 深圳先进技术研究院 Sodium titanate nanowire/graphene composite negative electrode material, and preparation method thereof
CN105720268A (en) * 2016-04-08 2016-06-29 辽宁大学 Lithium ion battery anode material and preparation method of lithium ion battery anode material
CN105845901A (en) * 2016-03-28 2016-08-10 辽宁大学 Lithium ion battery negative material Li4Ti5O12 / TiO2 / RGO 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
CN108134072A (en) * 2018-01-30 2018-06-08 中国科学院宁波材料技术与工程研究所 A kind of lithium titanate based composites and preparation method thereof
CN108529603A (en) * 2018-06-26 2018-09-14 西南交通大学 Alcohol heat-treats the method and graphene of graphene oxide
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
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
CN111312997A (en) * 2019-03-13 2020-06-19 北京纳米能源与系统研究所 Composite material and preparation method and application thereof
CN113394382A (en) * 2021-06-11 2021-09-14 北京化工大学 Titanium potassium phosphate @ carbon-redox graphene 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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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
CN105206810A (en) * 2015-09-16 2015-12-30 宁波南车新能源科技有限公司 Nanometer 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
CN105336940A (en) * 2015-10-20 2016-02-17 深圳先进技术研究院 Sodium titanate nanowire/graphene composite negative electrode material, and preparation method thereof
CN105845901A (en) * 2016-03-28 2016-08-10 辽宁大学 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
CN105720268A (en) * 2016-04-08 2016-06-29 辽宁大学 Lithium ion battery anode material and preparation method of lithium ion battery anode material
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
CN108134072A (en) * 2018-01-30 2018-06-08 中国科学院宁波材料技术与工程研究所 A kind of lithium titanate based composites 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
CN111312997A (en) * 2019-03-13 2020-06-19 北京纳米能源与系统研究所 Composite material and preparation method and application thereof
CN111312997B (en) * 2019-03-13 2021-07-13 北京纳米能源与系统研究所 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
CN113394382A (en) * 2021-06-11 2021-09-14 北京化工大学 Titanium potassium phosphate @ carbon-redox graphene material, preparation method thereof and potassium ion battery
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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