CN106328959A - Preparation method of TiO2-Graphene composite material - Google Patents

Preparation method of TiO2-Graphene composite material Download PDF

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Publication number
CN106328959A
CN106328959A CN201610671203.2A CN201610671203A CN106328959A CN 106328959 A CN106328959 A CN 106328959A CN 201610671203 A CN201610671203 A CN 201610671203A CN 106328959 A CN106328959 A CN 106328959A
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Prior art keywords
tio
graphene
preparation
composite
microwave
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赵新生
王敏
李建伟
魏永生
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Jiangsu Normal University
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Jiangsu Normal 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
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/0204—Non-porous and characterised by the material
    • H01M8/0223—Composites
    • 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
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—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
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
    • 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
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells
    • 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 preparation method of a TiO2-Graphene composite material. The method comprises the steps of preparing a graphene oxide (GO) solution from flaky graphite as a raw material; fully mixing 1-butyl-3-methylimidazolium tetrafluoroborate, glacial acetic acid and water, dropwise adding tetrabutyl titanate, carrying out magnetic stirring until the solution is bright white, carrying out ultrasonic treatment until the solution is colorless and transparent, carrying out treatment by using a microwave-assisted ionic heat method, washing an obtained TiO2 sample by deionized water and absolute ethyl alcohol for multiple times separately and drying for use; and respectively weighing different quantities of GO and TiO2 for fully mixing, carrying out homogeneous ultrasonic dispersion, carrying out treatment by using a microwave-assisted hydrothermal method, washing the obtained sample by the deionized water and the ethyl alcohol for multiple times separately, carrying out vacuum drying and then obtaining the TiO2-Graphene composite material of different ratios. According to the preparation method of the TiO2-Graphene composite material, the TiO2-Graphene composite material is obtained through microwave-assisted methods; the method is simple and easy to operate, high in reaction speed and short in synthesis time; and the obtained product is high in purity, good in repeatability, high in practicability and low in cost.

Description

TiO2The preparation method of-Graphene composite
Technical field
The invention belongs to field of fuel cell technology, relate to the preparation method of a kind of composite, particularly relate to one TiO2The preparation method of-Graphene composite.
Background technology
Proton Exchange Membrane Fuel Cells is by novel with the one that the chemical energy in oxidant is converted into electric energy for fuel TRT, has energy conversion efficiency high, and start-up temperature is low, the advantage such as quiet noiselessness, simple in construction, clean environment firendly, is The preferred electrical source of power of electric automobile, mobile electronic equipment and communication base station.
Catalyst is the critical material of Proton Exchange Membrane Fuel Cells, plays decisive to battery performance, life-span and cost Effect.At present, custom catalysts is that carbon carries Pt series, such as Pt/C, Pt-Ru/C etc., mainly with carbon dust Vulcan XC-72 for carrying Body.But, during fuel cell long-play, carbon carrier is susceptible to corrosion in strong acid, high potential environment, causes Metallic separates with carrier, the reunion of metallic, and the carbon dust reunited has a strong impact on material transferring.Urge to improve The resistance to corrosion of agent carrier, some metal-oxides such as SnO2、WO3、CeO2、TiO2Etc. being used as carrier material.Wherein, Because of TiO2There is stable chemical performance under strong acid environment, abundance, advantage with low cost, especially TiO2With noble metal it Between there is the characteristic of " strong interaction " so that it is become excellent fuel-cell catalyst carrier [S.Meenakshi, K.G.Nishanth.Electrochimica Acta,2014,135:52–59；Jianbing Zhu.Carbon,2014,72: 114-124；Samaneh Shahgaldi.Fuel,2015,150:645–655；Wang Z Y,Chen G,Xia D G,et al.Journal of Alloys and Compounds,2008,450:148-151；Hirakawa,Inoue M,Abe T.Electrochimica Acta,2010,55:5874-5880].But TiO2The surface area of carrier is little, conductive capability is weak, and TiO2Interphase interaction with carbon dust is the most weak, increases the resistance of catalyst, reduces the activity of catalyst.
Graphene is a kind of two-dimensional layer material, has good electric conductivity and chemical stability.But Graphene sheet The Van der Waals force that interlayer is more weak, causes lamella easily to be reunited, and specific surface area diminishes, and then have impact on its physicochemical characteristics, because of And need other materials compound to optimize its performance [Chemical Society Reviews, 2012,41 (2): 666-686]. At present, some are had about TiO2Patent [the CN102569761A of-Graphene composite；CN102553560A； CN102553559A；CN102976314A；CN105158295A；CN104998630A；CN104815637A； CN104437660A], by TiO2-Graphene composite is used for new forms of energy, field of new.Wherein, TiO2-Graphene Composite also present good performance [Ahmed G.El-Deen, Jae-Hwan as catalytic carrier Choi.Desalination,2015,361:53–64；Lei Zhao,Zhen-Bo Wang.Journal of Power Sources,2015,279:210-217].But existing TiO2Crystal growth lack preferred orientation, major part be specific surface area relatively Little chondritic, easily reunites, and is unfavorable for giving full play to TiO2Advantage respective with Graphene.
In view of problem above, the present invention proposes a kind of simplicity, quick, safe preparation method, prepares little crystal grain, height Scattered TiO2-Graphene composite is as the carrier of catalyst of fuel batter with proton exchange film, and this carrier has higher Stability, electric conductivity and electrochemical surface area, in catalyst field, there is extraordinary application prospect.
Summary of the invention
The technical problem to be solved is: provide a kind of TiO2The preparation method of-Graphene composite, can Improving the convenience of operation, method is simple and easy to operate, and response speed is fast, and generated time is short, and the product purity obtained is high, reappears Property is good, practical, low cost.
For solving above-mentioned technical problem, the present invention adopts the following technical scheme that
A kind of TiO2The preparation method of-Graphene composite, described preparation method includes:
Step 1., with flaky graphite as raw material, uses Hummer ' the s method improved, and prepares GO solution；
Step 2. takes 1-butyl-3 methyl imidazolium tetrafluoroborate [bmin] [BF4], glacial acetic acid and water be sufficiently mixed, then by Being added dropwise to butyl titanate, magnetic agitation presents brilliant white to solution, is then sonicated to water white transparency shape, uses microwave-assisted Ion full-boiled process, processes 25-40min, the TiO obtained at 180～200 DEG C2Sample is washed with deionized water and dehydrated alcohol respectively Wash for several times, dried for standby；
TiO2Presoma in acid condition, add [bmin] [BF4], use microwave-assisted ion full-boiled process, 180～ 25-40min has been reacted at 200 DEG C；
Step 3. takes GO and TiO of different quality respectively2Being sufficiently mixed, ultrasonic disperse is uniform, uses microwave-assisted hydro-thermal Method, processes 15～20min at 140-160 DEG C, the sample deionized water obtained, ethanol is washed respectively for several times, 80-100 10～12h it are vacuum dried, it is thus achieved that the TiO of different proportion at DEG C2The composite of-Graphene；This composite is by size At the mesoporous cubic body TiO of 70～80nm2It is evenly distributed on Graphene composition；
Ratio shared by Graphene is 10～80wt.%, and remaining is TiO2；Wherein, TiO2Form be cubical Jie Pore structure, and TiO2All it is dispersed in Graphene surface；
Using titanium source and GO is initial feed, with water, acetic acid, ionic liquid as reaction dissolvent, by microwave assisting method, obtains There is the cube TiO of meso-hole structure2With Graphene composite.
A kind of TiO2The preparation method of-Graphene composite, described preparation method includes:
Step 1. prepares GO solution with flaky graphite for raw material；
Step 2. takes 1-butyl-3 methyl imidazolium tetrafluoroborate, glacial acetic acid and water and is sufficiently mixed, then is added dropwise over metatitanic acid Four butyl esters, magnetic agitation presents brilliant white to solution, is then sonicated to water white transparency shape, uses at microwave-assisted ion full-boiled process Reason, the TiO obtained2Sample uses deionized water and absolute ethanol washing for several times respectively, dried for standby；
Step 3. takes GO and TiO of different quality respectively2Being sufficiently mixed, ultrasonic disperse is uniform, uses microwave-assisted hydro-thermal Method processes, and the sample deionized water obtained, ethanol is washed respectively for several times, obtains the TiO of different proportion after vacuum drying2- The composite of Graphene.
As a preferred embodiment of the present invention, the ratio shared by Graphene is 10～80wt.%, and remaining is TiO2； Wherein, TiO2Form be cubical meso-hole structure, and TiO2All it is dispersed in Graphene surface.
As a preferred embodiment of the present invention, using titanium source and GO is initial feed, is anti-with water, acetic acid, ionic liquid Answer solvent, by microwave assisting method, obtain the cube TiO with meso-hole structure2With Graphene composite.
As a preferred embodiment of the present invention, described composite be by size 70～80nm mesoporous cubic body TiO2It is evenly distributed on Graphene composition.
As in a preferred embodiment of the present invention, step 2, TiO2Presoma in acid condition, add [bmin][BF4], use microwave-assisted ion full-boiled process, at 180 DEG C, react 25min.
As in a preferred embodiment of the present invention, step 3, the temperature of microwave-hydrothermal method is 150 DEG C, and the response time is 15min。
As in a preferred embodiment of the present invention, step 3, the sample deionized water obtained, ethanol are washed respectively For several times, 10h it is vacuum dried at 80 DEG C, it is thus achieved that the TiO of different proportion2The composite of-Graphene.
The beneficial effects of the present invention is: the TiO that the present invention proposes2The preparation method of-Graphene composite, TiO2- Graphene composite is obtained by microwave assisting method, and method is simple and easy to operate, and response speed is fast, and generated time is short, and The product purity arrived is high, and favorable reproducibility is practical, low cost.It addition, need not add any hydrotropy during reaction Agent, additive, catalyst, whole course of reaction is nontoxic, harmless, pollution-free.The TiO of preparation under the method2Pattern is cube, Particle diameter less (70～80nm), and be evenly distributed.Using the composite of this series as after supported carrier noble metal, can be necessarily The degree of scatter of noble metal, and TiO in catalyst is improved in degree2And there is " strong interaction " between noble metal, prevent simultaneously Stop the corrosion of Graphene, shown as Proton Exchange Membrane Fuel Cells promoter carrier higher electrochemically stable Property and activity.
Accompanying drawing explanation
Fig. 1 is cubic block TiO prepared by embodiment one2Stereoscan photograph
Fig. 2 is cubic block TiO prepared by embodiment one2XRD figure spectrum
Fig. 3 is TiO prepared by embodiment one2The XRD figure spectrum of the composite nano materials of-Graphene
Fig. 4 is TiO prepared by embodiment one2The stereoscan photograph of-Graphene composite nano materials, amplifies 500 times
Fig. 5 is TiO prepared by embodiment one2The stereoscan photograph of-Graphene composite nano materials, amplifies 20000 Times
Fig. 6 is TiO of the present invention2The flow chart of the preparation method of-Graphene composite.
Detailed description of the invention
Describe the preferred embodiments of the present invention below in conjunction with the accompanying drawings in detail.
Embodiment one
Refer to Fig. 6, present invention is disclosed a kind of TiO2The preparation method of-Graphene composite, described preparation side Method includes:
Step 1., with flaky graphite as raw material, uses Hummer ' the s method improved, and prepares GO solution；
Step 2. takes 1-butyl-3 methyl imidazolium tetrafluoroborate [bmin] [BF4], glacial acetic acid and water be sufficiently mixed, then by Being added dropwise to butyl titanate, magnetic agitation presents brilliant white to solution, is then sonicated to water white transparency shape, uses microwave-assisted Ion full-boiled process, processes 25min, the TiO obtained at 180 DEG C2Sample uses deionized water and absolute ethanol washing for several times respectively, dry Dry stand-by；
TiO2Presoma in acid condition, add [bmin] [BF4], employing microwave-assisted ion full-boiled process, 180 DEG C Under reacted 25min；
Step 3. takes GO and TiO of different quality respectively2Being sufficiently mixed, ultrasonic disperse is uniform, uses microwave-assisted hydro-thermal Method, processes 15min at 150 DEG C, the sample deionized water obtained, ethanol is washed respectively for several times, be vacuum dried at 80 DEG C 10h, it is thus achieved that the TiO of different proportion2The composite of-Graphene (obtains the cube TiO with meso-hole structure2With Graphene composite)；This composite be by size 70～80nm mesoporous cubic body TiO2It is evenly distributed on Graphene is upper to be constituted；Ratio shared by Graphene is 10～80wt.%, and remaining is TiO2；Wherein, TiO2Form be vertical The meso-hole structure of cube, and TiO2All it is dispersed in Graphene surface；
Fig. 1 is cubic block TiO2Stereoscan photograph, as can be seen from Figure 2 TiO2For cubic, particle diameter be 70～ 80nm.Fig. 2 is the cubic block TiO of experimental procedure 2 preparation2XRD figure spectrum, as can be seen from Figure 2 TiO2Crystal formation be anatase Type.Fig. 3 is mesoporous TiO2Compose with the XRD figure of Graphene composite, the TiO that as can be seen from Figure 3 prepared by the present invention2With After Graphene is combined by microwave-assisted, TiO2Crystal formation is still Detitanium-ore-type.Fig. 4 to Fig. 5 is the scanning of this composite By these two figures, photo, can be seen that Graphene plays the effect of derivant, it is possible in the feelings not adding any template Under condition, mesoporous anatase TiO can be prepared2With Graphene nano composite material.
Embodiment two
The present embodiment TiO that be take GO Yu 80mg of 20mg different from embodiment one2Mixing, it is thus achieved that TiO2- Graphene composite, wherein Graphene content is 20%, and remaining is TiO2, other step and specific embodiment one phase With.
Embodiment three
The present embodiment TiO that be take GO Yu 70mg of 30mg different from embodiment one2Mixing, it is thus achieved that TiO2- Graphene composite, wherein Graphene content is 30%, and remaining is TiO2, other step is identical with embodiment one.
Embodiment four
The present embodiment TiO that be take GO Yu 60mg of 40mg different from embodiment one2Mixing, it is thus achieved that TiO2- Graphene composite, wherein Graphene content is 40%, and remaining is TiO2, other step is identical with embodiment one.
Embodiment five
The present embodiment TiO that be take GO Yu 50mg of 50mg different from embodiment one2Mixing, it is thus achieved that TiO2- Graphene composite, wherein Graphene content is 50%, and remaining is TiO2, other step is identical with embodiment one.
Embodiment six
The present embodiment TiO that be take GO Yu 40mg of 60mg different from embodiment one2Mixing, it is thus achieved that TiO2- Graphene composite, wherein Graphene content is 60%, and remaining is TiO2, other step is identical with embodiment one.
Embodiment seven
The present embodiment TiO that be take GO Yu 20mg of 80mg different from embodiment one2Mixing, it is thus achieved that TiO2- Graphene composite, wherein Graphene content is 80%, and remaining is TiO2, other step is identical with embodiment one.
In sum, the TiO that the present invention proposes2The preparation method of-Graphene composite, TiO2-Graphene is combined Material is obtained by microwave assisting method, and method is simple and easy to operate, and response speed is fast, and generated time is short, and the product purity obtained Height, favorable reproducibility, practical, low cost.It addition, need not add any cosolvent, additive, urge during reaction Agent, whole course of reaction is nontoxic, harmless, pollution-free.The TiO of preparation under the method2Pattern is cube, and particle diameter is less by (70 ～80nm), and be evenly distributed.Using the composite of this series as after supported carrier noble metal, can improve to a certain extent The degree of scatter of noble metal, and T iO in catalyst2And there is " strong interaction " between noble metal, prevent simultaneously The corrosion of Graphene, as Proton Exchange Membrane Fuel Cells promoter carrier show higher electrochemical stability and Activity.
Here description of the invention and application is illustrative, is not wishing to limit the scope of the invention to above-described embodiment In.The deformation of embodiments disclosed herein and change are possible, real for those skilled in the art The various parts with equivalence of replacing executing example are known.It should be appreciated by the person skilled in the art that without departing from the present invention Spirit or essential characteristics in the case of, the present invention can in other forms, structure, layout, ratio, and with other assembly, Material and parts realize.In the case of without departing from scope and spirit of the present invention, embodiments disclosed herein can be entered Other deformation of row and change.

Claims (8)

1. a TiO2The preparation method of-Graphene composite, it is characterised in that described preparation method includes:
Step 1., with flaky graphite as raw material, uses Hummer ' the s method improved, and prepares GO solution；
Step 2. takes 1-butyl-3 methyl imidazolium tetrafluoroborate [bmin] [BF4], glacial acetic acid and water is sufficiently mixed, more dropwise adds Entering butyl titanate, magnetic agitation presents brilliant white to solution, is then sonicated to water white transparency shape, uses microwave-assisted ion Full-boiled process, processes 25～40min, the TiO obtained at 180～200 DEG C2Sample is respectively with deionized water and absolute ethanol washing number Secondary, dried for standby；
TiO2Presoma in acid condition, add [bmin] [BF4], use microwave-assisted ion full-boiled process, 180 DEG C～200 25～40min have been reacted at DEG C；
Step 3. takes GO and TiO of different quality respectively2Being sufficiently mixed, ultrasonic disperse is uniform, uses microwave-assisted hydro-thermal method, Process 15～20min at 140～160 DEG C, the sample deionized water obtained, ethanol are washed for several times respectively, at 80～100 DEG C Vacuum drying 10～12h, it is thus achieved that the TiO of different proportion2The composite of-Graphene；This composite is 70 by size ～the mesoporous cubic body TiO of 80nm2It is evenly distributed on Graphene composition；Ratio shared by Graphene be 10～ 80wt.%, remaining is TiO2；Wherein, TiO2Form be cubical meso-hole structure, and TiO2All it is dispersed in Graphene surface；
Using titanium source and GO is initial feed, with water, acetic acid, ionic liquid as reaction dissolvent, by microwave assisting method, is had The cube TiO of meso-hole structure2With Graphene composite.
2. a TiO2The preparation method of-Graphene composite, it is characterised in that described preparation method includes:
Step 1. prepares GO solution with flaky graphite for raw material；
Step 2. takes 1-butyl-3 methyl imidazolium tetrafluoroborate, glacial acetic acid and water and is sufficiently mixed, then is added dropwise over metatitanic acid four fourth Ester, magnetic agitation presents brilliant white to solution, is then sonicated to water white transparency shape, uses microwave-assisted ion full-boiled process to process, The TiO obtained2Sample uses deionized water and absolute ethanol washing for several times respectively, dried for standby；
Step 3. takes GO and TiO of different quality respectively2Being sufficiently mixed, ultrasonic disperse is uniform, uses at microwave-assisted hydro-thermal method Reason, washs the sample deionized water obtained, ethanol respectively for several times, obtains the TiO of different proportion after vacuum drying2- The composite of Graphene.
TiO the most according to claim 22The preparation method of-Graphene composite, it is characterised in that:
In step 2, TiO2Presoma in acid condition, add [bmin] [BF4], use microwave-assisted ion full-boiled process, 25～40min have been reacted at 180 DEG C～200 DEG C.
TiO the most according to claim 22The preparation method of-Graphene composite, it is characterised in that:
In step 3, the ratio shared by Graphene is 10～80wt.%, and remaining is TiO2；Wherein, TiO2Form be cube Meso-hole structure, and TiO2All it is dispersed in Graphene surface.
TiO the most according to claim 22The preparation method of-Graphene composite, it is characterised in that:
In step 3, using titanium source and GO is initial feed, with water, acetic acid, ionic liquid as reaction dissolvent, by microwave assisting method, Obtain the cube TiO with meso-hole structure2With Graphene composite.
TiO the most according to claim 22The preparation method of-Graphene composite, it is characterised in that:
In step 3, described composite be by size 70～80nm mesoporous cubic body TiO2It is evenly distributed on Graphene Constitute.
TiO the most according to claim 22The preparation method of-Graphene composite, it is characterised in that:
In step 3, the temperature of microwave-hydrothermal method is 140～160 DEG C, and the response time is 15～20min.
TiO the most according to claim 22The preparation method of-Graphene composite, it is characterised in that:
In step 3, the sample deionized water obtained, ethanol are washed for several times respectively, at 80～100 DEG C be vacuum dried 10～ 12h, it is thus achieved that the TiO of different proportion2The composite of-Graphene.
CN201610671203.2A 2016-08-15 2016-08-15 Preparation method of TiO2-Graphene composite material Pending CN106328959A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
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Application publication date: 20170111

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