CN104009238A - Method for in-situ synthesis of compound of rutile TiO2 mesocrystal and graphene - Google Patents

Method for in-situ synthesis of compound of rutile TiO2 mesocrystal and graphene Download PDF

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Publication number
CN104009238A
CN104009238A CN201410276617.6A CN201410276617A CN104009238A CN 104009238 A CN104009238 A CN 104009238A CN 201410276617 A CN201410276617 A CN 201410276617A CN 104009238 A CN104009238 A CN 104009238A
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mesomorphic
graphene
graphene complex
rutile tio
tio
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魏明灯
蓝通斌
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Fuzhou University
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Fuzhou University
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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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention discloses a method for in-situ synthesis of compound of rutile TiO2 mesocrystal and graphene. A simple hydrothermal method is adopted to carry out in-situ synthesis on the compound of the rutile TiO2 mesocrystal and the graphene, and the compound of the rutile TiO2 mesocrystal and the grapheme is used for assembling lithium ion batteries. The method for the in-situ synthesis of the compound of the rutile TiO2 mesocrystal and the grapheme is simple in preparation, cost is low, energy consumption is low, repeatability is good, and the manufactured lithium ion batteries have high specific capacity and long-range cycling stability, show excellent multiplying power charge-discharge properties, and have wide commercial prospects.

Description

A kind of original position titania TiO 2the method of mesomorphic and graphene complex
Technical field
The invention belongs to electrode material preparation field, be specifically related to a kind of original position titania TiO 2the method of mesomorphic and graphene complex.
Background technology
Lithium ion battery is the green high-capacity environment-protecting battery occurring the nineties in 20th century, has a wide range of applications owing to having outstanding advantage.At present, lithium ion battery and critical material thereof have become science and technology and the industry focus paid close attention to countries in the world, and the Ye Shi Chinese government pays much attention to exploitation and one of energy of using, is successively put into national Long-and Medium-term Development planning.Especially the exploitation that is applicable to the lithium-ion-power cell of electric automobile (EV) and hybrid vehicle (HEV) becomes in recent years the most popular, development research field the most rapidly in new energy field especially.Industrial conventional negative material has lithium metal, material with carbon element, Li now 4ti 5o 12deng.But due to lithium metal with material with carbon element exists security performance hidden danger and high rate performance is poor and Li 4ti 5o 12the shortcomings such as synthetic difficulty, have limited its large-scale application.TiO 2it is one of the most popular lithium ion battery negative material of research at present.
Summary of the invention
The object of the present invention is to provide a kind of original position titania TiO 2the method of mesomorphic and graphene complex, its preparation method is simple, with low cost, energy consumption is low, favorable reproducibility, and obtained lithium ion battery has very high specific capacity and long-range cyclical stability, also show excellent rate charge-discharge performance, there is wide commercial promise.
For achieving the above object, the present invention adopts following technical scheme:
A kind of original position titania TiO 2mesomorphic and method graphene complex comprises the following steps:
(1) DBSA is scattered in salpeter solution;
(2) after uniform emulsion to be formed, drip graphene oxide solution, stir, finally splash into butyl titanate, continue to stir;
(3) through hydro-thermal reaction, centrifugal, washing, dry, make rutile TiO 2mesomorphic and graphene oxide compound;
(4) by rutile TiO 2mesomorphic and graphene oxide compound are dispersed in water, and after hydro-thermal reaction, centrifugal, washing, drying, obtain rutile TiO 2mesomorphic and graphene complex.
In step (1), the addition of DBSA is 0.5-5 mL; The concentration of salpeter solution is 0.5-6 mol/L.
In step (2), the addition of graphene oxide is 5-40 mg, and the addition of butyl titanate is 0.5-2 mL.
The described hydrothermal temperature of step (3) is 50-90 DEG C, and the reaction time is 3-72 h.
The described hydrothermal temperature of step (4) is 120-180 DEG C.
Described rutile TiO 2mesomorphic and graphene complex is used for assembling lithium ion battery: by rutile TiO 2mesomorphic and graphene complex, Kynoar and acetylene black are in mass ratio for 8:1:1 mixed grinding is evenly coated on Copper Foil, to be dried rear as negative pole, using lithium metal as positive pole, by LiPF 6/ EC-EMC-DMC solution, as electrolyte, is assembled into lithium ion battery in glove box.
Described LiPF 6liPF in/EC-EMC-DMC solution 6concentration be 1 mol/L, wherein the volume ratio of EC, EMC and DMC is 1:1:1.
Remarkable advantage of the present invention is:
(1) the invention provides a kind of original position titania TiO 2the method of mesomorphic and graphene complex, the method is simple to operate, with low cost, and energy consumption is low, and favorable reproducibility has good using value.
(2) the rutile TiO making 2mesomorphic and graphene complex are as the negative pole of lithium ion battery, the lithium ion battery that assembling obtains has very high specific capacity and long-range cyclical stability, in the time that current density is 3.4 A/g, charge and discharge cycles 1000 is enclosed Capacitance reserve more than 150 mA h/g, has superior long cycle performance; Meanwhile, it also shows excellent multiplying power discharging property, even its charge/discharge capacity also can be stabilized in 139.6 mA h/g in the time that current density is 6.8 A/g.
Brief description of the drawings
Fig. 1 is the prepared rutile TiO of embodiment 1 2mesomorphic and graphene complex scanning electron microscope (SEM) photograph and transmission electron microscope picture.
Fig. 2 is by prepared embodiment 1 rutile TiO 2the cycle performance curve (1C=170 mA/g) that the mesomorphic lithium ion battery being assembled into graphene complex discharges and recharges under different multiplying.
Embodiment
Embodiment 1
A kind of rutile TiO 2the preparation method of mesomorphic and graphene complex, comprises the following steps:
1) 0.68 mL DBSA is scattered in 70 mL 2 mol/L salpeter solutions;
2) after uniform emulsion to be formed, drip 2 mL graphene oxide solution (5 mg/mL), stir, finally splash into 0.68 mL butyl titanate, continue to stir;
3) gained mixed liquor is reacted to 48 h under 70 DEG C of water bath condition, take out, naturally cool to room temperature, centrifugation product, with alcohol water washing 5 times, dries, and makes rutile TiO 2mesomorphic and graphene oxide compound.
4) take 100 mg rutile TiO 2mesomorphic and graphene oxide compound is scattered in 35 mL water, packs reactor into, and in 140 DEG C of baking ovens, reaction 6 h, take out, naturally cool to room temperature, and centrifugation product, with alcohol water washing 3 times, is dried, and makes rutile TiO 2mesomorphic and graphene complex.
By gained rutile TiO 2mesomorphic and graphene complex is used for assembling lithium ion battery, and its assemble method comprises: by rutile TiO 2mesomorphic and graphene complex, Kynoar and acetylene black are coated on Copper Foil after evenly for 8:1:1 mixed grinding in mass ratio, after vacuumize as negative pole, using lithium metal as positive pole, by 1 mol/L LiPF 6/ EC-EMC-DMC(1:1:1, v/v/v) solution is as electrolyte, and in glove box, described lithium ion battery is made in assembling.
From scanning electron microscope (SEM) photograph, can find out rutile TiO 2mesomorphic one-tenth is cylindric, is made up of ultra-fine little crystal grain.From transmission electron microscope picture, can clearly find out rutile TiO 2mesomorphicly surrounded rutile TiO by ultra-thin graphene nanometer sheet 2mesomorphic size is in 100-200 nanometer.
Lithium ion battery charge and discharge cycles 1000 in the time that current density is 3.4 A/g of the present embodiment assembling is enclosed Capacitance reserve more than 150 mA h/g, has superior long cycle performance; Meanwhile, it also shows excellent multiplying power discharging property, even its charge/discharge capacity also can be stabilized in 139.6 mA h/g in the time that current density is 6.8 A/g.
Embodiment 2
A kind of rutile TiO 2the preparation method of mesomorphic and graphene complex, comprises the following steps:
1) 1.035 mL DBSA are scattered in 70 mL 2 mol/L salpeter solutions;
2) after uniform emulsion to be formed, drip 3 mL graphene oxide solution (5 mg/mL), stir, finally splash into 0.68 mL butyl titanate, continue to stir;
3) gained mixed liquor is reacted to 48 h under 70 DEG C of water bath condition, take out, naturally cool to room temperature, centrifugation product, with alcohol water washing 5 times, dries, and makes rutile TiO 2mesomorphic and graphene oxide compound.
4) take 100 mg rutile TiO 2mesomorphic and graphene oxide compound is scattered in 35 mL water, packs reactor into, and in 140 DEG C of baking ovens, reaction 6 h, take out, naturally cool to room temperature, and centrifugation product, with alcohol water washing 3 times, is dried, and makes rutile TiO 2mesomorphic and graphene complex.
By gained rutile TiO 2mesomorphic and graphene complex is used for assembling lithium ion battery, and its assemble method comprises: by rutile TiO 2mesomorphic and graphene complex, Kynoar and acetylene black are coated on Copper Foil after evenly for 8:1:1 mixed grinding in mass ratio, after vacuumize as negative pole, using lithium metal as positive pole, by 1 mol/L LiPF 6/ EC-EMC-DMC(1:1:1, v/v/v) solution is as electrolyte, and in glove box, described lithium ion battery is made in assembling.
Lithium ion battery charge and discharge cycles 1000 in the time that current density is 3.4 A/g of the present embodiment assembling is enclosed Capacitance reserve more than 150 mA h/g, has superior long cycle performance; Meanwhile, it also shows excellent multiplying power discharging property, even its charge/discharge capacity also can be stabilized in 139.6 mA h/g in the time that current density is 6.8 A/g.
Embodiment 3
A kind of rutile TiO 2the preparation method of mesomorphic and graphene complex, comprises the following steps:
1) 0.68 mL DBSA is scattered in 70 mL 4 mol/L salpeter solutions;
2) after uniform emulsion to be formed, drip 2 mL graphene oxide solution (5 mg/mL), stir, finally splash into 0.68 mL butyl titanate, continue to stir;
3) gained mixed liquor is reacted to 72 h under 70 DEG C of water bath condition, take out, naturally cool to room temperature, centrifugation product, with alcohol water washing 5 times, dries, and makes rutile TiO 2mesomorphic and graphene oxide compound.
4) take 100 mg rutile TiO 2mesomorphic and graphene oxide compound is scattered in 35 mL water, packs reactor into, and in 140 DEG C of baking ovens, reaction 6 h, take out, naturally cool to room temperature, and centrifugation product, with alcohol water washing 3 times, is dried, and makes rutile TiO 2mesomorphic and graphene complex.
By gained rutile TiO 2mesomorphic and graphene complex is used for assembling lithium ion battery, and its assemble method comprises: by rutile TiO 2mesomorphic and graphene complex, Kynoar and acetylene black are coated on Copper Foil after evenly for 8:1:1 mixed grinding in mass ratio, after vacuumize as negative pole, using lithium metal as positive pole, by 1 mol/L LiPF 6/ EC-EMC-DMC(1:1:1, v/v/v) solution is as electrolyte, and in glove box, described lithium ion battery is made in assembling.
Lithium ion battery charge and discharge cycles 1000 in the time that current density is 3.4 A/g of the present embodiment assembling is enclosed Capacitance reserve more than 150 mA h/g, has superior long cycle performance; Meanwhile, it also shows excellent multiplying power discharging property, even its charge/discharge capacity also can be stabilized in 139.6 mA h/g in the time that current density is 6.8 A/g.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.

Claims (10)

1. an original position titania TiO 2the method of mesomorphic and graphene complex, is characterized in that: adopt simple hydro thermal method original position to prepare rutile TiO 2mesomorphic and graphene complex.
2. original position titania TiO according to claim 1 2the method of mesomorphic and graphene complex, is characterized in that: comprise the following steps:
(1) DBSA is scattered in salpeter solution;
(2) after uniform emulsion to be formed, drip graphene oxide solution, stir, finally splash into butyl titanate, continue to stir;
(3) through hydro-thermal reaction, centrifugal, washing, dry, make rutile TiO 2mesomorphic and graphene oxide compound;
(4) by rutile TiO 2mesomorphic and graphene oxide compound are dispersed in water, and after hydro-thermal reaction, centrifugal, washing, drying, obtain rutile TiO 2mesomorphic and graphene complex.
3. original position titania TiO according to claim 2 2the method of mesomorphic and graphene complex, is characterized in that: in step (1), the addition of DBSA is 0.5-5 mL; The concentration of salpeter solution is 0.5-6 mol/L.
4. original position titania TiO according to claim 2 2the method of mesomorphic and graphene complex, is characterized in that: in step (2), the addition of graphene oxide is 5-40 mg, and the addition of butyl titanate is 0.5-2 mL.
5. original position titania TiO according to claim 2 2the method of mesomorphic and graphene complex, is characterized in that: the described hydrothermal temperature of step (3) is 50-90 DEG C, and the reaction time is 3-72 h.
6. original position titania TiO according to claim 2 2the method of mesomorphic and graphene complex, is characterized in that: the described hydrothermal temperature of step (4) is 120-180 DEG C.
7. the rutile TiO that the method for claim 1 makes 2mesomorphic and graphene complex.
8. the rutile TiO that the method for claim 1 makes 2the application of mesomorphic and graphene complex, is characterized in that: described rutile TiO 2mesomorphic and graphene complex is used for assembling lithium ion battery.
9. rutile TiO according to claim 8 2the application of mesomorphic and graphene complex, is characterized in that: the assemble method of described lithium ion battery comprises: by rutile TiO 2mesomorphic and graphene complex, Kynoar and acetylene black are in mass ratio for 8:1:1 mixed grinding is evenly coated on Copper Foil, to be dried rear as negative pole, using lithium metal as positive pole, by LiPF 6/ EC-EMC-DMC solution, as electrolyte, is assembled into lithium ion battery in glove box.
10. rutile TiO according to claim 8 2the application of mesomorphic and graphene complex, is characterized in that: described LiPF 6liPF in/EC-EMC-DMC solution 6concentration be 1 mol/L, wherein the volume ratio of EC, EMC and DMC is 1:1:1.
CN201410276617.6A 2014-06-20 2014-06-20 Method for in-situ synthesis of compound of rutile TiO2 mesocrystal and graphene Pending CN104009238A (en)

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CN106207118A (en) * 2016-07-26 2016-12-07 中南大学 A kind of regulate and control the method for nano titanium oxide pattern of graphene coated and the product of preparation thereof and application
CN106328959A (en) * 2016-08-15 2017-01-11 江苏师范大学 Preparation method of TiO2-Graphene composite material
CN106370858A (en) * 2016-08-20 2017-02-01 福建师范大学 Potential addressing mode-based double tumor marker photoelectric detection method
CN106450237A (en) * 2016-12-08 2017-02-22 福州大学 Preparation and application of lithium-sulfur battery positive electrode composite material
CN107565114A (en) * 2017-08-30 2018-01-09 北京理工大学 A kind of binder free anode material of lithium-ion battery and preparation method thereof
CN109637696A (en) * 2018-10-29 2019-04-16 徐冬 A kind of high-effective conductive agent
CN113178569A (en) * 2021-03-22 2021-07-27 黑龙江工业学院 Preparation method of pillared layer carrier semiconductor type natural graphite composite lithium battery negative electrode material

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Cited By (13)

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CN105810926B (en) * 2016-04-07 2018-08-17 福州大学 A kind of method of simple regulation and control mesomorphic TiO2 construction unit sizes
CN105810926A (en) * 2016-04-07 2016-07-27 福州大学 Method for simply controlling size of mesocrystal TiO2 construction unit
CN106207118A (en) * 2016-07-26 2016-12-07 中南大学 A kind of regulate and control the method for nano titanium oxide pattern of graphene coated and the product of preparation thereof and application
CN106207118B (en) * 2016-07-26 2018-09-11 中南大学 A kind of method of nano-titanium dioxide pattern of regulation and control graphene coated and its product of preparation and application
CN106328959A (en) * 2016-08-15 2017-01-11 江苏师范大学 Preparation method of TiO2-Graphene composite material
CN106370858A (en) * 2016-08-20 2017-02-01 福建师范大学 Potential addressing mode-based double tumor marker photoelectric detection method
CN106370858B (en) * 2016-08-20 2017-11-07 福建师范大学 A kind of photoelectric detecting method of double tumor markerses based on current potential addressing mode
CN106450237B (en) * 2016-12-08 2019-04-05 福州大学 A kind of preparation and application of anode composite material of lithium sulfur battery
CN106450237A (en) * 2016-12-08 2017-02-22 福州大学 Preparation and application of lithium-sulfur battery positive electrode composite material
CN107565114A (en) * 2017-08-30 2018-01-09 北京理工大学 A kind of binder free anode material of lithium-ion battery and preparation method thereof
CN107565114B (en) * 2017-08-30 2020-12-15 北京理工大学 Binderless sodium ion battery negative electrode material and preparation method thereof
CN109637696A (en) * 2018-10-29 2019-04-16 徐冬 A kind of high-effective conductive agent
CN113178569A (en) * 2021-03-22 2021-07-27 黑龙江工业学院 Preparation method of pillared layer carrier semiconductor type natural graphite composite lithium battery negative electrode material

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