CN104148045A - Arc process-based graphene/titanium dioxide composite material preparation method - Google Patents
Arc process-based graphene/titanium dioxide composite material preparation method Download PDFInfo
- Publication number
- CN104148045A CN104148045A CN201410404557.1A CN201410404557A CN104148045A CN 104148045 A CN104148045 A CN 104148045A CN 201410404557 A CN201410404557 A CN 201410404557A CN 104148045 A CN104148045 A CN 104148045A
- Authority
- CN
- China
- Prior art keywords
- arc discharge
- graphene
- discharge device
- titanium dioxide
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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 a helium 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 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 greatly specific area.Graphene and other materials carry out compound tense, can prepare the composite of excellent performance.By compound to Graphene and semi-conducting material, in the time that 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, 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 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, make nano titanium oxide and Graphene reaction in dispersion liquid 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, 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, 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 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 is carrying out, after a large amount of creative works, having 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 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;
Pass into the mist of helium and air to 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.
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 helium 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, pass into cooling water to described arc discharge device.
Alternatively, described titanium dioxide sample 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 to prepare by the preparation method of above-mentioned Graphene/composite titania material.
Beneficial effect of the present invention is:
1, method safety.The present invention adopts air and helium as mist, has replaced 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 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, starts to making Graphene/composite titania material required time short 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 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.
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 real protection scope of the present invention formed to any type of any restriction.
Embodiment 1
Take 0.6g TiO
2powder, is pressed into the pressed compact that diameter is 15mm with mould, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with negative electrode and the anode taking graphite as electrode, 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, 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 0.6g TiO
2powder, is pressed into the pressed compact that diameter is 15mm with mould, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with negative electrode and the anode taking graphite as electrode, 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, 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 0.6g TiO
2powder, is pressed into the pressed compact that diameter is 15mm with mould, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with negative electrode and the anode taking graphite as electrode, 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, 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 0.6g TiO
2powder, is pressed into the pressed compact that diameter is 15mm with mould, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with negative electrode and the anode taking graphite as electrode, 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, 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 0.6g TiO
2powder, is pressed into the pressed compact that diameter is 15mm with mould, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with negative electrode and the anode taking graphite as electrode, 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, 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 0.4g TiO
2powder, is pressed into the pressed compact that diameter is 10mm with mould, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with negative electrode and the anode taking graphite as electrode, 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, 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 1.0g TiO
2powder, is pressed into the pressed compact that diameter is 20mm with mould, and this pressed compact is put into arc discharge device, and this arc discharge device is provided with negative electrode and the anode taking graphite as electrode, 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, 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 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;
To the mist that passes into helium 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 helium 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, passes into cooling water to described arc discharge device.
7. preparation method according to claim 1 and 2, is characterized in that, described titanium dioxide sample 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410404557.1A CN104148045B (en) | 2014-08-15 | 2014-08-15 | Based on the preparation method of the graphene/titania composite material of arc process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410404557.1A CN104148045B (en) | 2014-08-15 | 2014-08-15 | Based on the preparation method of the graphene/titania composite material of arc process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104148045A true CN104148045A (en) | 2014-11-19 |
| CN104148045B CN104148045B (en) | 2016-02-03 |
Family
ID=51873784
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410404557.1A Expired - Fee Related CN104148045B (en) | 2014-08-15 | 2014-08-15 | Based on the preparation method of the graphene/titania composite material of arc process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104148045B (en) |
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 |
| 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 |
-
2014
- 2014-08-15 CN CN201410404557.1A patent/CN104148045B/en not_active Expired - Fee Related
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104148045B (en) | 2016-02-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Dong et al. | Visible-light responsive PDI/rGO composite film for the photothermal catalytic degradation of antibiotic wastewater and interfacial water evaporation | |
| Feng et al. | Synthetic routes of the reduced graphene oxide | |
| Hu et al. | One-pot synthesis of step-scheme Bi2S3/porous g-C3N4 heterostructure for enhanced photocatalytic performance | |
| Liao et al. | Enhanced photocatalytic and photoelectrochemical activities of SnO2/SiC nanowire heterostructure photocatalysts | |
| Guo et al. | Z-scheme g-C3N4/Bi2O2 [BO2 (OH)] heterojunction for enhanced photocatalytic CO2 reduction | |
| Qian et al. | A stable and highly efficient visible-light-driven hydrogen evolution porous CdS/WO3/TiO2 photocatalysts | |
| Liu et al. | Template-free preparation of non-metal (B, P, S) doped g-C3N4 tubes with enhanced photocatalytic H2O2 generation | |
| Cheng et al. | Multi-walled carbon nanotubes act as charge transport channel to boost the efficiency of hole transport material free perovskite solar cells | |
| Chen et al. | TiO2 nanotube arrays co-loaded with Au nanoparticles and reduced graphene oxide: Facile synthesis and promising photocatalytic application | |
| Mao et al. | Modification of surface properties and enhancement of photocatalytic performance for g-C3N4 via plasma treatment | |
| CN106944116A (en) | Carbonitride/titanium dioxide nanoplate array heterojunction photochemical catalyst and preparation method | |
| Gao et al. | Freestanding atomically-thin cuprous oxide sheets for improved visible-light photoelectrochemical water splitting | |
| Yao et al. | Enhanced photoelectrochemical performance of hydrogenated ZnO hierarchical nanorod arrays | |
| Ting et al. | Efficiency improvement of the DSSCs by building the carbon black as bridge in photoelectrode | |
| CN104313549B (en) | A kind of preparation method with the graphene-based film of self-cleaning function | |
| Hou et al. | Interfacial hydrothermal synthesis of SnO2 nanorods towards photocatalytic degradation of methyl orange | |
| Wei et al. | Hydrogenated TiO2 nanotube arrays with enhanced photoelectrochemical property for photocathodic protection under visible light | |
| Pan et al. | In situ construction of g-C3N4/TiO2 heterojunction films with enhanced photocatalytic activity over magnetic-driven rotating frame | |
| Du et al. | Amorphous carbon inhibited TiO2 phase transition in aqueous solution and its application in photocatalytic degradation of organic dye | |
| Shen et al. | 2D/2D/3D architecture Z‑scheme system for simultaneous H2 generation and antibiotic degradation | |
| Jiang et al. | Plasmon Ag decorated 3D urchinlike N-TiO2− x for enhanced visible-light-driven photocatalytic performance | |
| Velusamy et al. | Investigate the suitability of g-C3N4 nanosheets ornamented with BiOI nanoflowers for photocatalytic dye degradation and PEC water splitting | |
| Umadevi et al. | Enhanced photocatalytic, antimicrobial activity and photovoltaic characteristics of fluorine doped TiO2 synthesized under ultrasound irradiation | |
| Zhong et al. | Solvothermal preparation of Ag nanoparticles sensitized TiO2 nanotube arrays with enhanced photoelectrochemical performance | |
| CN102709399B (en) | Manufacturing method of high-efficiency nano antenna solar battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160203 Termination date: 20200815 |