CN104148045B - Based on the preparation method of the graphene/titania composite material of arc process - Google Patents
Based on the preparation method of the graphene/titania composite material of arc process Download PDFInfo
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- CN104148045B CN104148045B CN201410404557.1A CN201410404557A CN104148045B CN 104148045 B CN104148045 B CN 104148045B CN 201410404557 A CN201410404557 A CN 201410404557A CN 104148045 B CN104148045 B CN 104148045B
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Abstract
The present invention relates to a kind of preparation method of the graphene/titania composite material based on arc process, this preparation method comprises the following steps: take titanium dioxide and put into the negative electrode of arc discharge device and the centre of anode electrode; The mist of helium and air is passed into this arc discharge device; Opening this arc discharge device makes it discharge, and regulates size of current and control the reaction time; Electric discharge terminates rear obtained graphene/titania composite material.The present invention overcomes the danger of discharging in hydrogen atmosphere, arc discharge makes the reaction speed of raw material accelerate simultaneously, and generated time is short.The technique of the inventive method is simple, easy to operate, practical.
Description
Technical field
The present invention relates to inorganic composite materials field, specifically a kind of preparation method of the graphene/titania composite material based on arc process and the material for preparing thereof.
Background technology
Graphene is a kind of stable two-dimension plane structure, and therefore, Graphene has high electric conductivity and thermal conductance, high specific strength and great specific area.Graphene and other materials carry out compound tense, can prepare the composite of excellent performance.By Graphene and semi-conducting material compound, when material is irradiated by light, light induced electron can be injected in Graphene, effectively prevents the compound in light induced electron and hole, thus improves photocatalysis efficiency, significantly improves the performance of catalysis material.
Titanium dioxide (TiO
2) be a kind of semi-conducting material, there are fabulous photoelectric conversion capacity, long-time stability and be close to the inorganic material of the excellent properties such as nontoxic, have a wide range of applications in fields such as photovoltaic solar cell, light-catalyzed reaction, photocatalytic degradation, sewage disposals, but there is the slower shortcoming of degrading activity in it.So people are to TiO
2photochemical catalyst has carried out study on the modification widely, comprising the compound of the deposition of catalyst surface noble metal, semiconductor light-catalyst, ion doping, the photoactivate of photochemical catalyst and form central hole structure etc.Many documents also report and adopt new carbon such as CNT, C60, class graphitic carbon material, Graphene etc. to form composite with photochemical catalyst hydridization, enhance the photocatalysis performance of material to organic matter, pollutant.
Number of patent application 201010590547.3 discloses a kind of graphene/nanometer titanium dioxide compound and preparation method thereof, by nano titanium oxide and graphene dispersion in a certain proportion of water/ethanolic solution, make the nano titanium oxide in dispersion liquid and Graphene reaction by pressurizeing and heating up.
Number of patent application 201110225465.3 discloses a kind of graphene/mesoporous titanium dioxide visible light catalyst and preparation method thereof, is joined by graphene oxide in glacial acetic acid, and ultrasonic disperse obtains the dispersion liquid of graphene oxide; In the dispersion liquid of graphene oxide, add titanium source, prepare Graphene/mesoporous TiO 2 nano compounded visible light catalyst by hydro-thermal method.
Number of patent application 201210582986.9 discloses a kind of preparation method of graphene/titanium dioxide photocatalyst, graphene oxide is joined the mixed solution of water and ethanol, being added drop-wise to by this mixed solution is dissolved with in the chloroform of butyl titanate again, final mixed liquor water heating kettle is reacted, obtained graphene/titanium dioxide photocatalyst.
Number of patent application 201310287749.4 discloses the preparation method of a kind of Graphene and composite titania material, presoma containing titanium ion is dissolved in absolute ethyl alcohol, be mixed with solution, add graphene oxide solution again, deposition, drying, then Graphene and composite titania material can be obtained by hydro-thermal method.
The preparation method of current Graphene mainly contains micromechanics stripping method, chemical vapour deposition technique, electronation graphene oxide method and solvent-thermal method etc., and the preparation method of Graphene and composite titania material mainly hydro-thermal method and solvent-thermal method etc., as above-mentioned prior art all adopts hydro-thermal method.But these methods have its respective limitation:
1, micromechanics stripping method, this method technique is simple, with low cost, but wastes time and energy, and the product size dimension of preparation is wayward, and poor repeatability is difficult to extensive preparation.
2, chemical vapour deposition technique, this method can prepare the large-area Graphene of high-quality, can meet the requirement that high-quality graphene is prepared in scale, but cost is higher, complex process.
3, electronation graphene oxide method, general adopts the reducing agent redox graphenes such as hydrazine, then with titanium dioxide compound, the reducing agent adopted generally has toxicity, not environmentally, limits its application prospect.
4, solvent-thermal method, generated time is long, complex process, and production efficiency is low.
Therefore, provide that a kind of preparation time is short, simple to operate, the preparation method of Graphene that technique environmental protection, preparation efficiency are high and composite titania material, the suitability for industrialized production for this composite is very favourable.
Summary of the invention
In order to solve the problems of the technologies described above, provide that a kind of preparation time is short, simple to operate, technique environmental protection, graphene/titania composite material that preparation efficiency is high preparation method, the present inventor, after carrying out a large amount of creative works, completes the present invention.
The invention provides a kind of preparation method of the graphene/titania composite material based on arc process, the method comprises the following steps:
Take titanium dioxide sample, put into arc discharge device, be provided with negative electrode and the anode of making electrode with graphite in described arc discharge device, described titanium dioxide sample is placed on the centre of described negative electrode and anode electrode;
The mist of helium and air is passed into described arc discharge device;
Open described arc discharge device, regulate size of current, described arc discharge device is discharged;
Electric discharge terminates, obtained described graphene/titania composite material.
Further, described titanium dioxide sample is the titania powder of 0.4g ~ 1.0g, described titania powder is put into mould and suppresses, and obtains the pressed compact that diameter is 10mm ~ 20mm, described pressed compact is placed on the centre of described negative electrode and anode electrode.
Preferably, described titanium dioxide sample is the titania powder of 0.6g, described titania powder is put into mould and suppresses, and obtains the pressed compact that diameter is 15mm, described pressed compact is placed on the centre of described negative electrode and anode electrode.
Further, in described mist, the pressure of described helium is 500torr ~ 2000torr.
Further, setting electric current is 80A ~ 200A, and the reaction time is 10s ~ 200s.
Further, open described arc discharge device in the process of electric discharge end, pass into cooling water to described arc discharge device.
Alternatively, described titanium dioxide sample can be rutile, also can be anatase.
The present invention also provides a kind of graphene/titania composite material, and this graphene/titania composite material is prepared by the preparation method of above-mentioned graphene/titania composite material.
Beneficial effect of the present invention is:
1, method safety.The present invention adopts air and helium as mist, instead of inflammable and explosive hydrogen, and the security of the inventive method is increased.
2, reaction speed is fast, and generated time is short.In the present invention, there is arc discharge in two graphite electrodes under certain voltage, and carbon atom is reset and formed Graphene, and arc discharge makes reaction temperature raise rapidly simultaneously, can make TiO instantaneously
2become molten condition, Graphene enters in the lattice of titanium dioxide, obtained graphene/titania composite material within tens of second.
After having reacted, cooling velocity is fast, and in several minutes, temperature is down to room temperature, short to obtained graphene/titania composite material required time from reaction.
3, product purity is high, favorable reproducibility.In the process of arc discharge, the plasma that electric arc produces is pure, can not introduce any impurity, and therefore obtained product purity is high.In addition, in the inventive method, the electric current of arc discharge and reaction time all can accurately control, the stability of product and favorable reproducibility.
4, practical, cost is low.The technique of the inventive method is simple, and easy to operate, in addition, without any need for cosolvent, additive, catalyst, cost is low, and whole course of reaction is nontoxic, harmless, pollution-free.
Detailed description of the invention
Below by specific embodiment, the present invention is described in detail, should be understood that, these detailed description of the invention are only used for exemplifying the present invention, not forms any type of any restriction to real protection scope of the present invention.
Embodiment 1
Take 0.6gTiO
2powder, is pressed into mould the pressed compact that diameter is 15mm, this pressed compact is put into arc discharge device, and it is negative electrode and the anode of electrode that this arc discharge device is provided with graphite, by TiO
2pressed compact is placed in the middle of negative electrode and anode; Pass into cooling water to arc discharge device, and pass into 500Torr helium; Open arc discharge device, arranging electric current is 80A, and the reaction time is 100s, and arc discharge device is discharged; Electric discharge terminates, powered-down, regulates pressure, takes out obtained graphene/titania composite material.
Embodiment 2
Take 0.6gTiO
2powder, is pressed into mould the pressed compact that diameter is 15mm, this pressed compact is put into arc discharge device, and it is negative electrode and the anode of electrode that this arc discharge device is provided with graphite, by TiO
2pressed compact is placed in the middle of negative electrode and anode; Pass into cooling water to arc discharge device, and pass into 1500Torr helium; Open arc discharge device, arranging electric current is 120A, and the reaction time is 60s, and arc discharge device is discharged; Electric discharge terminates, powered-down, regulates pressure, takes out obtained graphene/titania composite material.
Embodiment 3
Take 0.6gTiO
2powder, is pressed into mould the pressed compact that diameter is 15mm, this pressed compact is put into arc discharge device, and it is negative electrode and the anode of electrode that this arc discharge device is provided with graphite, by TiO
2pressed compact is placed in the middle of negative electrode and anode; Pass into cooling water to arc discharge device, and pass into 2000Torr helium; Open arc discharge device, arranging electric current is 200A, and the reaction time is 15s, and arc discharge device is discharged; Electric discharge terminates, powered-down, regulates pressure, takes out obtained graphene/titania composite material.
Embodiment 4
Take 0.6gTiO
2powder, is pressed into mould the pressed compact that diameter is 15mm, this pressed compact is put into arc discharge device, and it is negative electrode and the anode of electrode that this arc discharge device is provided with graphite, by TiO
2pressed compact is placed in the middle of negative electrode and anode; Pass into cooling water to arc discharge device, and pass into 1000Torr helium; Open arc discharge device, arranging electric current is 120A, and the reaction time is 150s, and arc discharge device is discharged; Electric discharge terminates, powered-down, regulates pressure, takes out obtained graphene/titania composite material.
Embodiment 5
Take 0.6gTiO
2powder, is pressed into mould the pressed compact that diameter is 15mm, this pressed compact is put into arc discharge device, and it is negative electrode and the anode of electrode that this arc discharge device is provided with graphite, by TiO
2pressed compact is placed in the middle of negative electrode and anode; Pass into cooling water to arc discharge device, and pass into 1000Torr helium; Open arc discharge device, arranging electric current is 80A, and the reaction time is 200s, and arc discharge device is discharged; Electric discharge terminates, powered-down, regulates pressure, takes out obtained graphene/titania composite material.
Embodiment 6
Take 0.4gTiO
2powder, is pressed into mould the pressed compact that diameter is 10mm, this pressed compact is put into arc discharge device, and it is negative electrode and the anode of electrode that this arc discharge device is provided with graphite, by TiO
2pressed compact is placed in the middle of negative electrode and anode; Pass into cooling water to arc discharge device, and pass into 1000Torr helium; Open arc discharge device, arranging electric current is 100A, and the reaction time is 150s, and arc discharge device is discharged; Electric discharge terminates, powered-down, regulates pressure, takes out obtained graphene/titania composite material.
Embodiment 7
Take 1.0gTiO
2powder, is pressed into mould the pressed compact that diameter is 20mm, this pressed compact is put into arc discharge device, and it is negative electrode and the anode of electrode that this arc discharge device is provided with graphite, by TiO
2pressed compact is placed in the middle of negative electrode and anode; Pass into cooling water to arc discharge device, and pass into 2000Torr helium; Open arc discharge device, arranging electric current is 200A, and the reaction time is 10s, and arc discharge device is discharged; Electric discharge terminates, powered-down, regulates pressure, takes out obtained graphene/titania composite material.
Should be understood that, the purposes of above-described embodiment is only the present invention is described and is not intended to limit the scope of the invention.Simultaneously; also should be understood that; after having read technology contents of the present invention; those skilled in the art can be under the premise without departing from the principles of the invention; do suitably to change to the raw material in the technical scheme of invention and process route; realize final technology of preparing, these all equivalents fall within the protection domain that the application's appended claims limits equally.
Claims (7)
1. based on a preparation method for the graphene/titania composite material of arc process, it is characterized in that, the method comprises the following steps:
Take titanium dioxide sample, put into arc discharge device, be provided with negative electrode and the anode of making electrode with graphite in described arc discharge device, described titanium dioxide sample is placed on the centre of described negative electrode and anode electrode;
The mist of helium and air is passed in described arc discharge device;
Open described arc discharge device, regulate size of current, described arc discharge device is discharged; Wherein, setting electric current is 80A ~ 200A, and the reaction time is 10s ~ 200s;
Electric discharge terminates, obtained described graphene/titania composite material.
2. preparation method according to claim 1, it is characterized in that, described titanium dioxide sample is the titania powder of 0.4g ~ 1.0g, described titania powder is put into mould suppress, obtain the pressed compact that diameter is 10mm ~ 20mm, described pressed compact is placed on the centre of described negative electrode and anode electrode.
3. preparation method according to claim 2, it is characterized in that, described titanium dioxide sample is the titania powder of 0.6g, described titania powder is put into mould and suppresses, obtain the pressed compact that diameter is 15mm, described pressed compact is placed on the centre of described negative electrode and anode electrode.
4. preparation method according to claim 1 and 2, is characterized in that, in described mist, the pressure of described helium is 500torr ~ 2000torr.
5. preparation method according to claim 1 and 2, is characterized in that, opens described arc discharge device in the process of electric discharge end, passes into cooling water to described arc discharge device.
6. preparation method according to claim 1 and 2, is characterized in that, described titanium dioxide sample is rutile or anatase.
7. a graphene/titania composite material, is characterized in that, described graphene/titania composite material is obtained by the preparation method described in any one of claim 1 to 6.
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| CN101717083A (en) * | 2009-12-29 | 2010-06-02 | 北京大学 | Graphene and preparation method thereof |
| CN102153076A (en) * | 2011-05-04 | 2011-08-17 | 上海大学 | Method for preparing graphene with high crystallinity |
| CN102350334A (en) * | 2011-08-08 | 2012-02-15 | 江苏大学 | Graphene/mesoporous titanium dioxide visible light catalyst and preparation method |
| CN102553559A (en) * | 2010-12-08 | 2012-07-11 | 财团法人纺织产业综合研究所 | Graphene/nanometer titanium dioxide compound and preparation method thereof |
| CN103028387A (en) * | 2012-12-28 | 2013-04-10 | 聊城大学 | Preparation method of graphene/titanium dioxide photocatalyst |
| CN103337611A (en) * | 2013-07-10 | 2013-10-02 | 厦门大学 | Preparation method of graphene-titanium dioxide composite material |
| CN103695869A (en) * | 2013-12-20 | 2014-04-02 | 上海中电振华晶体技术有限公司 | Preparation method of graphene film |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717083A (en) * | 2009-12-29 | 2010-06-02 | 北京大学 | Graphene and preparation method thereof |
| CN102553559A (en) * | 2010-12-08 | 2012-07-11 | 财团法人纺织产业综合研究所 | Graphene/nanometer titanium dioxide compound and preparation method thereof |
| CN102153076A (en) * | 2011-05-04 | 2011-08-17 | 上海大学 | Method for preparing graphene with high crystallinity |
| CN102350334A (en) * | 2011-08-08 | 2012-02-15 | 江苏大学 | Graphene/mesoporous titanium dioxide visible light catalyst and preparation method |
| CN103028387A (en) * | 2012-12-28 | 2013-04-10 | 聊城大学 | Preparation method of graphene/titanium dioxide photocatalyst |
| CN103337611A (en) * | 2013-07-10 | 2013-10-02 | 厦门大学 | Preparation method of graphene-titanium dioxide composite material |
| CN103695869A (en) * | 2013-12-20 | 2014-04-02 | 上海中电振华晶体技术有限公司 | Preparation method of graphene film |
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