CN104577131A - Preparation method of graphite-TiO2-B composite material - Google Patents

Preparation method of graphite-TiO2-B composite material Download PDF

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Publication number
CN104577131A
CN104577131A CN201510022135.2A CN201510022135A CN104577131A CN 104577131 A CN104577131 A CN 104577131A CN 201510022135 A CN201510022135 A CN 201510022135A CN 104577131 A CN104577131 A CN 104577131A
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graphene
tio
composite material
preparation
tio2
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周忠福
张晶晶
王敬峰
王清露
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • 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

Abstract

The invention relates to a preparation method of a graphite-TiO2-B composite material. The method comprises the following steps: (1) preparing graphite oxide by utilizing a Hummers method, and then preparing graphene by utilizing a hot swelling method; (2) preparing bud-shaped TiO2-B from titanium source and additives by utilizing a hydrothermal method; and (3) physically stirring the graphene and the TiO2-B at the room temperature, and mixing the graphene and the TiO2-B to obtain a graphene-coating bud-shaped TiO2-B composite material. The composite material is the graphene-coating bud-shaped TiO2-B, and the size of the bud is about 400nm to 500nm. The preparation method of the graphene-coating bud-shaped TiO2-B composite material has advantages of being simple and low in cost, the prepared graphene-coating bud-shaped TiO2-B composite material can be widely applied to a lithium battery negative electrode material and is good in rate capacity and circulating stability, and the chemical performance can be remarkably improved.

Description

A kind of Graphene-TiO 2the preparation method of-B composite material
Technical field
The invention belongs to field of composite material preparation, relate to a kind of Graphene-TiO 2the preparation method of-B composite material.
Background technology
Graphene is from 2004 by after the reports such as the professor Geim of Univ Manchester UK, and the physical and chemical performance because of its uniqueness causes to be paid close attention to widely.Two dimension (2D) the cycle honeycomb lattice structure that Graphene is made up of carbon hexatomic ring, it is the elementary cell building other dimension carbon-based material.Graphene has a lot of excellent structures and characteristics, and such as high specific area, large electron mobility, good thermal conductivity etc., can it can be used as performance enhancement phase and other compound to carry out compound, prepare the composite material of excellent performance.
TiO 2-B is mutually initial to be found in 1980 by Marchand etc.; Banfield etc. pass through K subsequently 2ti 4o 9the method such as ion-exchange, heat treatment successfully prepare TiO 2-B.TiO 2-B is a kind of metastable crystal formation, a kind of metasable state titanium oxide homogeneity variant little, more loosely organized than the density of rutile and anatase, its design feature is par excellence to there is the feature parallel channels along [010] direction in crystal structure, when being used on lithium battery, be conducive to the combination of lithium ion in passage and diffusion.Compared to the crystal formation such as anatase and rutile, there is higher reversible specific capacity.
People's reported first such as Kobayashi TiO 2the synthesis of-B nano particle, the diameter of nano particle is 3-6nm; The people such as Armostrong have synthesized TiO first 2-B nano wire, diameter is 20-40nm; The people such as Liu have prepared the TiO with multilevel hierarchy 2-B, prepared material is by very thin TiO 2-B nanometer sheet is formed.
At present, TiO 2the microstructure of-B material is still constantly being optimized and is improving, no matter be nano wire, and the TiO of sheet or multilevel hierarchy 2-B, their surface area is less, in the application of lithium battery, can by restriction to a certain extent.
Chinese patent publication No. CN102437321 name is called Graphene-TiO 2(B) nanometer tube composite materials and preparation method thereof patent discloses a kind of Graphene and TiO 2(B) composite material and preparation method, it adopts sol-gel process to synthesize graphene oxide and TiO 2(B) plural gel, its pattern is the TiO of load on graphene layer 2nanotube; Chinese patent publication No. CN102600823B name is called that a kind of preparation method's of graphene/titania composite material patent discloses a kind of Graphene and TiO 2the preparation method of composite material, it adopts microwave radiation technology combustion method, by microwave heating, prepares Graphene and TiO 2composite material.Chinese patent publication No. CN101937985B name is called that a kind of graphene/titanium dioxide lithium ion battery cathode material and preparation method's patent discloses a kind of Graphene and TiO 2lithium ion battery negative material and preparation method, it adopts method graphene oxide and titanium source combined, and prepares Graphene and TiO by the method for In-situ reaction 2composite material.These preparation methods are mainly limited to hydro-thermal in-situ synthesis, are generally graphite oxide to be adopted the reducing agent reduction such as hydrazine, then with TiO 2compound.Reducing agent generally all has certain toxicity, and not environmentally, production efficiency is lower simultaneously, and cost is high, required equipment more complicated, and preparation time is relatively long, is unfavorable for that industrialization is applied on a large scale.
Adopt Graphene and petal shape TiO 2-B Material cladding, TiO 2-B has and is conducive to Li +the channel design of transmission, makes Li +at TiO 2embedding in-B and deviate from relatively easy, can show excellent fast charging and discharging ability.Based on this, TiO 2-B is than the TiO of other forms 2stored energy capacitance to exceed a lot.But because TiO 2conductivity own is bad, causes application to be subject to great restriction.And between graphene sheet layer, there is stronger Van der Waals force, there is the shortcoming easily occurring to reunite.By by TiO 2-beta particle is modified on graphene film, effectively can stop the reunion of Graphene.Like this, this kind of composite material not only can keep Graphene and TiO 2the primary characteristic of-B, also can produce new cooperative effect.When it uses as lithium cell cathode material, can bulk effect be overcome, significantly improve chemical property.
Summary of the invention
For the defect that prior art exists, the object of the present invention is to provide a kind of Graphene-TiO 2the preparation method of-B composite material, is applied on lithium cell cathode material and can significantly improves chemical property.
For achieving the above object, the present invention adopts following technical scheme:
A kind of Graphene-TiO 2the preparation method of-B composite material, the titania structure in this composite products is petal shape TiO 2-B, the method comprises the following steps:
(1) preparation of Graphene: take graphite powder as raw material, adopt Hummers legal system to obtain graphite oxide, thermal expansion obtains Graphene;
(2) petal shape TiO 2the preparation of-B: titanium source and auxiliary agent are put into beaker and stir and obtain mixed liquor, then mixed liquor is transferred in autoclave, react 4h ~ 24h at 150 DEG C, naturally cool to room temperature; Repeatedly wash with ethanol and deionized water after centrifugation, dry in an oven, the powder of drying is placed on 300 DEG C ~ 400 DEG C sintering 2h ~ 4h in Muffle furnace, cooling obtains petal shape TiO naturally 2-B material;
(3) Graphene and TiO 2the preparation of-B composite material: take TiO 2-B and Graphene, be dissolved in ethanol water respectively, is made into the mixed solution of certain mass concentration and ultrasonic; After two kinds of solution mixing after ultrasonic, in stirred at ambient temperature, dry in an oven, obtain Graphene-TiO 2-B composite material.
Further, the titanium source in described step (2) is TiCl 3, auxiliary agent is ethylene glycol and deionized water, TiCl 3, ethylene glycol and deionized water volume ratio be 1:(10 ~ 30): 1.
Further, the titanium source in described step (2) can also be TiCl 4, auxiliary agent selects ethylene glycol and ammoniacal liquor, TiCl 4, ethylene glycol and ammoniacal liquor volume ratio be 1:80:2.
Further, the mixed solution mass concentration in described step (3) is 1g/L, and ethanol used in ethanol water and the volume ratio of deionized water are 1:1.Ultrasonic time is 10min ~ 30min.The mix and blend time is 24h ~ 36h.Baking temperature lower than 100 DEG C, time 24h.
Compared with prior art, the present invention has following outstanding substantive distinguishing features and significant advantage:
Graphene-TiO prepared by this method 2-B composite material, wherein titanium dioxide component is for having petal shape TiO 2-B(bronze ore deposit), pattern is graphene coated petal shape TiO 2-B, wherein petal shape TiO 2the diameter of-B nano material is at 400nm ~ 500nm.Graphene coated petal shape TiO prepared by the present invention 2the advantages such as the preparation of-B composite material has technique simply, with low cost, can be widely used on lithium cell cathode material, have good high rate performance and cyclical stability, can significantly improve chemical property.
Accompanying drawing explanation
Fig. 1 is TiO 2x-ray diffraction spectrum (XRD) figure of-B.
Fig. 2 is TiO 2scanning electron microscopy (SEM) figure of-B.
Fig. 3 is Graphene and TiO 2scanning electron microscopy (SEM) figure of-B composite material.
Fig. 4 is TiO 2transmission electron microscope (TEM) figure of-B.
Fig. 5 is Graphene and TiO 2transmission electron microscope (TEM) figure of-B composite material.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
embodiment 1
A kind of Graphene-TiO 2the preparation method of-B composite material, the method comprises the following steps:
(1) preparation of Graphene
Take graphite powder as raw material, adopt Hummers method, i.e. NaNO 3join in the concentrated sulfuric acid, add graphite powder and potassium permanganate after dissolving completely, be obtained by reacting glassy yellow system further, after filtration drying, obtain graphite oxide, then by tube furnace, prepare Graphene through thermal expansion.
(2) petal shape TiO 2the preparation of-B
By 4mlTiCl 3, beaker put into by 4ml deionized water and 40ml ethylene glycol, stirs 10min.Mixed liquor is transferred in 50ml autoclave, react 6h at 150 DEG C, naturally cool to room temperature.Centrifugation, repeatedly washs with ethanol and deionized water.Then dry 8h at 60 DEG C, the powder of drying is placed on 400 DEG C of sintering 2h in Muffle furnace, cooling obtains petal shape TiO naturally 2-B material.
(3) Graphene and TiO 2the preparation of-B composite material
Weigh the TiO of 100mg 2-B is dissolved in the mixed solvent of 50ml ethanol, 50ml deionized water, ultrasonic 10min; Be dissolved in the mixed solvent of 5ml ethanol, 5ml deionized water with the Graphene of electronic balance weighing 10mg, ultrasonic 10min.Continue ultrasonic 10min again, stirred at ambient temperature 24h by after two kinds of solution mixing after ultrasonic, in 60 DEG C of baking ovens, dry 24h, obtains composite material.
embodiment 2
(1) preparation method of Graphene is with (1) step in embodiment 1.
(2) petal shape TiO 2the preparation of-B
4mlTiCl 3, 4ml deionized water at room temperature stirs, and adds 120ml ethylene glycol, stirs 10min, is transferred to by mixed liquor in 150ml autoclave, react 4h, naturally cool to room temperature at 150 DEG C.Repeatedly wash with ethanol and deionized water after centrifugation.Dry 8h at 60 DEG C, is placed on 300 DEG C of sintering 4h in Muffle furnace, naturally cools, obtain petal shape TiO by the powder of drying 2-B material.
(3) Graphene and TiO 2the preparation of-B composite material is with (3) step in embodiment 1.
embodiment 3
(1) preparation method of Graphene is with (1) step in embodiment 1.
(2) petal shape TiO 2the preparation of-B
By 1.0mlTiCl 4be dissolved in 80ml ethylene glycol, at room temperature stir 2h, add 2mL ammoniacal liquor (25wt%) afterwards, stir 10min.Mixed liquor is transferred in 100ml autoclave, react 24h at 150 DEG C, naturally cool to room temperature.Repeatedly wash with ethanol and deionized water after centrifugation.Dry 8h at 100 DEG C, is placed in Muffle furnace 350 DEG C sintering 2h, naturally cools, obtain petal shape TiO by the powder of drying 2-B material.
(3) Graphene and TiO 2the preparation of-B composite material is with (3) step in embodiment 1.
As shown in Figure 1, petal shape TiO 2the XRD spectra of-B can be found out, product is TiO 2-B(bronze ore deposit) structure; By Fig. 2 petal shape TiO 2the scanning electron microscope (SEM) photograph of-B can be found out, material presents the petal shape of comparatively rule, is of a size of 400nm ~ 500nm; By Fig. 3 Graphene and TiO 2the scanning electron microscope (SEM) photograph of-B composite material can be found out, TiO 2-B is coated on Graphene uniformly; By Fig. 4 TiO 2the transmission electron microscope picture of-B verifies TiO further 2the petal shape structure of-B; By Fig. 5 Graphene and TiO 2the transmission electron microscope picture of-B composite material can be found out, the TiO of Graphene organically coated 400 ~ 500nm 2-B.

Claims (7)

1. a Graphene-TiO 2the preparation method of-B composite material, is characterized in that, the titania structure in this composite products is petal shape TiO 2-B, the method comprises the following steps:
1) preparation of Graphene: take graphite powder as raw material, adopt Hummers legal system to obtain graphite oxide, thermal expansion obtains Graphene;
2) petal shape TiO 2the preparation of-B: titanium source and auxiliary agent are put into beaker and stir and obtain mixed liquor, then mixed liquor is transferred in autoclave, react 4h ~ 24h at 150 DEG C, naturally cool to room temperature; Repeatedly wash with ethanol and deionized water after centrifugation, dry in an oven, the powder of drying is placed on 300 DEG C ~ 400 DEG C sintering 2h ~ 4h in Muffle furnace, cooling obtains petal shape TiO naturally 2-B material;
3) Graphene and TiO 2the preparation of-B composite material: take TiO 2-B and Graphene, be dissolved in ethanol water respectively, is made into the mixed solution of certain mass concentration and ultrasonic; After two kinds of solution mixing after ultrasonic, in stirred at ambient temperature, dry in an oven, obtain Graphene-TiO 2-B composite material.
2. Graphene-TiO according to claim 1 2the preparation method of-B composite material, is characterized in that, described step 2) in titanium source be TiCl 3, auxiliary agent is ethylene glycol and deionized water, TiCl 3, ethylene glycol and deionized water volume ratio be 1:(10 ~ 30): 1.
3. Graphene-TiO according to claim 1 2the preparation method of-B composite material, is characterized in that, described step 2) in titanium source be TiCl 4, auxiliary agent selects ethylene glycol and ammoniacal liquor, TiCl 4, ethylene glycol and ammoniacal liquor volume ratio be 1:80:2.
4. Graphene-TiO according to claim 1 2the preparation method of-B composite material, is characterized in that, the mixed solution mass concentration in described step 3) is 1g/L, and ethanol used in ethanol water and the volume ratio of deionized water are 1:1.
5. Graphene-TiO according to claim 1 2the preparation method of-B composite material, is characterized in that, in described step 3), ultrasonic time is 10min ~ 30min.
6. Graphene-TiO according to claim 1 2the preparation method of-B composite material, is characterized in that, in described step 3), the mix and blend time is 24h ~ 36h.
7. Graphene-TiO according to claim 1 2the preparation method of-B composite material, is characterized in that, the baking temperature in described step 3) lower than 100 DEG C, time 24h.
CN201510022135.2A 2015-01-16 2015-01-16 Preparation method of graphite-TiO2-B composite material Pending CN104577131A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106356523A (en) * 2016-10-13 2017-01-25 华中科技大学 Preparation method of titanium dioxide sodium-ion battery cathode material and product thereof
CN106492776A (en) * 2016-11-02 2017-03-15 吉林大学 One kind prepares TiO2The method of graphene composite material
CN107785539A (en) * 2016-08-25 2018-03-09 中国科学院金属研究所 Sodium-ion battery TiO2The preparation method of/graphene composite negative pole
CN108574098A (en) * 2018-05-16 2018-09-25 华南师范大学 A kind of nanometer titanium dioxide-coated graphite lithium ion battery negative material and preparation method thereof
CN108918448A (en) * 2018-06-28 2018-11-30 河南省肿瘤医院 A kind of preparation method based on the enhanced enzyme biological sensing material of nanogold
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
CN114349054A (en) * 2021-12-23 2022-04-15 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of flower-bud-shaped molybdenum sulfide-titanium dioxide-B composite material, product and application thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN107785539A (en) * 2016-08-25 2018-03-09 中国科学院金属研究所 Sodium-ion battery TiO2The preparation method of/graphene composite negative pole
CN106356523A (en) * 2016-10-13 2017-01-25 华中科技大学 Preparation method of titanium dioxide sodium-ion battery cathode material and product thereof
CN106356523B (en) * 2016-10-13 2019-05-31 华中科技大学 A kind of preparation method and products thereof of titanium dioxide anode material of lithium-ion battery
CN106492776A (en) * 2016-11-02 2017-03-15 吉林大学 One kind prepares TiO2The method of graphene composite material
CN108574098A (en) * 2018-05-16 2018-09-25 华南师范大学 A kind of nanometer titanium dioxide-coated graphite lithium ion battery negative material and preparation method thereof
CN108918448A (en) * 2018-06-28 2018-11-30 河南省肿瘤医院 A kind of preparation method based on the enhanced enzyme biological sensing material of nanogold
CN108918448B (en) * 2018-06-28 2020-10-02 河南省肿瘤医院 Preparation method of nano-gold-based enhanced enzyme biosensing material
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
CN114349054A (en) * 2021-12-23 2022-04-15 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of flower-bud-shaped molybdenum sulfide-titanium dioxide-B composite material, product and application thereof

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Application publication date: 20150429