CN104148043A - Arc process-based graphene/titanium dioxide composite material preparation method - Google Patents
Arc process-based graphene/titanium dioxide composite material preparation method Download PDFInfo
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- CN104148043A CN104148043A CN201410403477.4A CN201410403477A CN104148043A CN 104148043 A CN104148043 A CN 104148043A CN 201410403477 A CN201410403477 A CN 201410403477A CN 104148043 A CN104148043 A CN 104148043A
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- arc discharge
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Abstract
The invention relates to an arc process-based graphene/titanium dioxide composite material preparation method. The preparation method comprises the following steps: weighing titanium dioxide, and putting the weighed titanium dioxide between a cathode and an anode of an arc discharge apparatus; introducing an argon and air mixed gas into the arc discharge apparatus; starting the arc discharge apparatus to discharge, adjusting the current size, controlling the reaction time; and ending the discharge to prepare the graphene/titanium dioxide composite material. The method overcomes the discharge danger in hydrogen atmosphere, accelerates the reaction speed of raw materials through arc discharge, and has a short synthetic time. The method has the advantages of simple technology, convenient operation and strong practicality.
Description
Technical field
The present invention relates to inorganic composite materials field, specifically a kind of preparation method of the Graphene/composite titania material based on arc process and preparation-obtained material 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 greatly specific area.Graphene and other materials carry out compound tense, can prepare the composite of excellent performance.Graphene and semi-conducting material is compound, and when material is irradiated by light, light induced electron can be injected in Graphene, effectively prevents the compound of light induced electron and hole, thereby improves photocatalysis efficiency, significantly improves the performance of catalysis material.
Titanium dioxide (TiO
2) be a kind of semi-conducting material, there is fabulous photoelectric conversion capacity, long-time stability and be close to the inorganic material of the excellent properties such as nontoxic, in fields such as photovoltaic solar cell, light-catalyzed reaction, photocatalytic degradation, sewage disposals, have a wide range of applications, 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 ion doping, the photoactivate of compound, the photochemical catalyst of the deposition of catalyst surface noble metal, semiconductor light-catalyst and form central hole structure etc.Many documents have also reported that employing new carbon such as CNT, C60, class graphitic carbon material, Graphene etc. and photochemical catalyst hydridization form composite, have strengthened 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, nano titanium oxide and Graphene are scattered in a certain proportion of water/ethanolic solution, by pressurizeing and heating up, make nano titanium oxide and Graphene in dispersion liquid react.
Number of patent application 201110225465.3 discloses a kind of graphene/mesoporous titanium dioxide visible light catalyst and preparation method thereof, and graphene oxide is joined in glacial acetic acid, and ultrasonic dispersion obtains the dispersion liquid of graphene oxide; In the dispersion liquid of graphene oxide, add titanium source, by hydro-thermal method, prepare Graphene/mesoporous TiO 2 nano compounded visible light catalyst.
Number of patent application 201210582986.9 discloses a kind of preparation method of Graphene/titanium dioxide optical catalyst, graphene oxide is joined to the mixed solution of water and ethanol, again this mixed solution is added drop-wise in the chloroform that is dissolved with butyl titanate, final mixed liquor is reacted with water heating kettle, make Graphene/titanium dioxide optical catalyst.
Number of patent application 201310287749.4 discloses the preparation method of a kind of Graphene and composite titania material, the presoma that contains titanium ion is dissolved in absolute ethyl alcohol, be mixed with solution, add again graphene oxide solution, deposition, dry, then can obtain Graphene and composite titania material by hydro-thermal method.
The preparation method of Graphene mainly contains micromechanics stripping method, chemical vapour deposition technique, electronation graphene oxide method and solvent-thermal method etc. at present, and the preparation method of Graphene and composite titania material is mainly hydro-thermal method and solvent-thermal method etc., as above-mentioned prior art all adopts hydro-thermal method.But these methods have its limitation separately:
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 be prepared 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, generally adopts the reducing agent redox graphenes such as hydrazine, more compound with titanium dioxide, and the reducing agent adopting generally has toxicity, and not environmental protection has limited its application prospect.
4, solvent-thermal method, generated time is long, complex process, production efficiency is low.
Therefore, the Graphene that provide that a kind of preparation time is short, simple to operate, technique environmental protection, preparation efficiency is high and the preparation method of composite titania material, be very favourable for the suitability for industrialized production of this composite.
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, the preparation method of technique environmental protection, Graphene/composite titania material that preparation efficiency is high, the inventor, after carrying out a large amount of creative works, has completed the present invention.
The preparation method who the invention provides a kind of Graphene/composite titania 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 with graphite, making electrode in described arc discharge device, described titanium dioxide sample is placed on the centre of described negative electrode and anode electrode;
To described arc discharge device, pass into the mist of argon gas and air;
Open described arc discharge device, regulate size of current, make described arc discharge device electric discharge;
Electric discharge finishes, and makes described Graphene/composite titania material.
Further, the titania powder that described titanium dioxide sample is 0.4g～1.0g, puts into mould by described titania powder and suppresses, and obtains the pressed compact that diameter is 10mm～20mm, described pressed compact is placed on to the centre of described negative electrode and anode electrode.
Preferably, the titania powder that described titanium dioxide sample is 0.6g, puts into mould by described titania powder and suppresses, and obtains the pressed compact that diameter is 15mm, described pressed compact is placed on to the centre of described negative electrode and anode electrode.
Further, in described mist, the pressure of described argon gas is 500torr～2000torr.
Further, setting electric current is 80A～200A, and the reaction time is 10s～200s.
Further, open described arc discharge device to the process of electric discharge end, to described arc discharge device, pass into cooling water.
Alternatively, described titania powder can be rutile, can be also anatase.
The present invention also provides a kind of Graphene/composite titania material, and this Graphene/composite titania material is that the preparation method by above-mentioned Graphene/composite titania material prepares.
Beneficial effect of the present invention is:
1, method safety.The present invention adopts air and argon gas as mist, has replaced inflammable and explosive hydrogen, and the security of this 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 raises rapidly reaction temperature simultaneously, can make TiO in moment
2become molten condition, Graphene enters in the lattice of titanium dioxide, in tens of seconds, makes Graphene/composite titania material.
After having reacted, cooling velocity is fast, and in several minutes, temperature is down to room temperature, from reaction, starts to making Graphene/composite titania material required time short.
3, product purity is high, favorable reproducibility.In the process of arc discharge, the mist passing into is pure clean, can not introduce any impurity, and the product purity therefore making is high.In addition, in the inventive method, the electric current of arc discharge and reaction time all can accurately be controlled, the stability of product and favorable reproducibility.
4, practical, cost is low.The technique of the inventive method is simple, easy to operate, and in addition, without any need for cosolvent, additive, catalyst, cost is low, and whole course of reaction is nontoxic, harmless, pollution-free.
The specific embodiment
Below by specific embodiment, the present invention is described in detail, should be understood that, these specific embodiment are only used for exemplifying the present invention, not real protection scope of the present invention formed to any type of any restriction.
Embodiment 1
Take 0.6gTiO
2powder, is pressed into mould the pressed compact that diameter is 15mm, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with take negative electrode and the anode that graphite is electrode, by TiO
2pressed compact is placed in the middle of negative electrode and anode; To arc discharge device, pass into cooling water, and pass into 500Torr argon gas; Open arc discharge device, it is 80A that electric current is set, and the reaction time is 100s, makes arc discharge device electric discharge; Electric discharge finishes, and powered-down regulates pressure, takes out the Graphene/composite titania material making.
Embodiment 2
Take 0.6gTiO
2powder, is pressed into mould the pressed compact that diameter is 15mm, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with take negative electrode and the anode that graphite is electrode, by TiO
2pressed compact is placed in the middle of negative electrode and anode; To arc discharge device, pass into cooling water, and pass into 1500Torr argon gas; Open arc discharge device, it is 120A that electric current is set, and the reaction time is 60s, makes arc discharge device electric discharge; Electric discharge finishes, and powered-down regulates pressure, takes out the Graphene/composite titania material making.
Embodiment 3
Take 0.6gTiO
2powder, is pressed into mould the pressed compact that diameter is 15mm, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with take negative electrode and the anode that graphite is electrode, by TiO
2pressed compact is placed in the middle of negative electrode and anode; To arc discharge device, pass into cooling water, and pass into 2000Torr argon gas; Open arc discharge device, it is 200A that electric current is set, and the reaction time is 15s, makes arc discharge device electric discharge; Electric discharge finishes, and powered-down regulates pressure, takes out the Graphene/composite titania material making.
Embodiment 4
Take 0.6gTiO
2powder, is pressed into mould the pressed compact that diameter is 15mm, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with take negative electrode and the anode that graphite is electrode, by TiO
2pressed compact is placed in the middle of negative electrode and anode; To arc discharge device, pass into cooling water, and pass into 1000Torr argon gas; Open arc discharge device, it is 120A that electric current is set, and the reaction time is 150s, makes arc discharge device electric discharge; Electric discharge finishes, and powered-down regulates pressure, takes out the Graphene/composite titania material making.
Embodiment 5
Take 0.6gTiO
2powder, is pressed into mould the pressed compact that diameter is 15mm, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with take negative electrode and the anode that graphite is electrode, by TiO
2pressed compact is placed in the middle of negative electrode and anode; To arc discharge device, pass into cooling water, and pass into 1000Torr argon gas; Open arc discharge device, it is 80A that electric current is set, and the reaction time is 200s, makes arc discharge device electric discharge; Electric discharge finishes, and powered-down regulates pressure, takes out the Graphene/composite titania material making.
Embodiment 6
Take 0.4gTiO
2powder, is pressed into mould the pressed compact that diameter is 10mm, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with take negative electrode and the anode that graphite is electrode, by TiO
2pressed compact is placed in the middle of negative electrode and anode; To arc discharge device, pass into cooling water, and pass into 1000Torr argon gas; Open arc discharge device, it is 100A that electric current is set, and the reaction time is 150s, makes arc discharge device electric discharge; Electric discharge finishes, and powered-down regulates pressure, takes out the Graphene/composite titania material making.
Embodiment 7
Take 1.0gTiO
2powder, is pressed into mould the pressed compact that diameter is 20mm, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with take negative electrode and the anode that graphite is electrode, by TiO
2pressed compact is placed in the middle of negative electrode and anode; To arc discharge device, pass into cooling water, and pass into 2000Torr argon gas; Open arc discharge device, it is 200A that electric current is set, and the reaction time is 10s, makes arc discharge device electric discharge; Electric discharge finishes, and powered-down regulates pressure, takes out the Graphene/composite titania material making.
Should be understood that, the purposes of above-described embodiment is only the present invention to be described but not to be intended to and limits 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; raw material and process route in the technical scheme of invention are made to appropriate change; realize final technology of preparing, within these all equivalents fall within the protection domain that the application's appended claims limits equally.
Claims (8)
1. a preparation method for the Graphene/composite titania material based on arc process, 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 with graphite, making electrode in described arc discharge device, described titanium dioxide sample is placed on the centre of described negative electrode and anode electrode;
To the mist that passes into argon gas and air in described arc discharge device;
Open described arc discharge device, regulate size of current, make described arc discharge device electric discharge;
Electric discharge finishes, and makes described Graphene/composite titania 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 to be suppressed, obtain the pressed compact that diameter is 10mm～20mm, described pressed compact is placed on to the centre of described negative electrode and anode electrode.
3. preparation method according to claim 2, it is characterized in that the titania powder that described titanium dioxide sample is 0.6g is put into mould by described titania powder and suppressed, obtain the pressed compact that diameter is 15mm, described pressed compact is placed on to 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 argon gas is 500torr～2000torr.
5. preparation method according to claim 1 and 2, is characterized in that, setting electric current is 80A～200A, and the reaction time is 10s～200s.
6. preparation method according to claim 1 and 2, is characterized in that, opens described arc discharge device to the process of electric discharge end, to described arc discharge device, passes into cooling water.
7. preparation method according to claim 1 and 2, is characterized in that, described titania powder can be rutile, can be also anatase.
8. Graphene/composite titania material, is characterized in that, described Graphene/composite titania material is to make by the preparation method described in claim 1 to 7 any one.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106475083A (en) * | 2016-09-08 | 2017-03-08 | 东北大学秦皇岛分校 | The preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993060A (en) * | 2009-08-19 | 2011-03-30 | 中国科学院金属研究所 | Method for massively preparing graphene with excellent electrical conductivity and thermal stability |
| 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 |
| US20140154597A1 (en) * | 2012-12-04 | 2014-06-05 | Fahs Stagemyer Llc | Fuel Cells Based on Precise Energy Separation |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993060A (en) * | 2009-08-19 | 2011-03-30 | 中国科学院金属研究所 | Method for massively preparing graphene with excellent electrical conductivity and thermal stability |
| 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 |
| US20140154597A1 (en) * | 2012-12-04 | 2014-06-05 | Fahs Stagemyer Llc | Fuel Cells Based on Precise Energy Separation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106475083A (en) * | 2016-09-08 | 2017-03-08 | 东北大学秦皇岛分校 | The preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor |
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