CN102531063A - Graphene load tungsten trioxide (WO3) nanowire composite material and preparation method thereof - Google Patents
Graphene load tungsten trioxide (WO3) nanowire composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene load tungsten trioxide (WO3) nanowire composite material and a preparation method thereof, which belong to the field of new materials. The nano composite material has a one-dimensional composite structure and a two-dimensional nano composite structure, the diameter of a WO3 nanowire is 10-30 nanometers, the length of the WO3 nanowire is 50-600 nanometers, and the WO3 nanowire penetrates through or is distributed on the inner layer or the surface of a layer-shaped grapheme main material. The preparation method comprises utilizing a two-dimensional grapheme as an auxiliary material and sodium tungstate as a tungsten source, generating the WO3 nanowire through a hydrothermal synthesis method, then mixing the WO3 nanowire with graphite oxide dispersing solution, and then obtaining the graphene load WO3 nanowire composite material by means of photocatalytic reduction. The preparation process is simple, reagents are cheap, large-scale preparation is facilitated, and simultaneously an environment-friendly preparation method is provided for reduction of graphite oxide and formation of the nano composite material.
Description
Technical field
The invention belongs to novel material and preparing technical field thereof, relate to a kind of graphene-supported WO
3Nano wire matrix material and preparation method thereof.
Technical background
Nano composite material is because the designability of its excellent comprehensive performances, particularly its performance is widely used in fields such as chemistry, optics and electricity.In recent years, nano composite material more and more obtains paying attention to.
Tungsten oxide 99.999 is typical transition metal oxide as a kind of n N-type semiconductorN.Tungsten oxide 99.999 is except as catalysis, electrochromism, electrode materials and the solar absorptive material, also has the character of air-sensitive, temperature-sensitive and semiconductor material such as pressure-sensitive.Tungsten oxide 99.999 can be applied in fields such as air-sensitive sensing, photochemical catalysis, photoconduction and ultracapacitor.Compare with traditional tungsten sill, tungsten oxide nano has bigger specific surface area, bigger surfactivity and stronger adsorptive power, has prospect widely in the functional materials Application Areas.
Graphene (graphene) is the two-dimensional nanostructure that the monolayer carbon atom is formed, and has that excellent electricity is led, thermal conductance and a mechanical property, and big specific surface area and absorption property.Utilize lamellar graphite alkene as material of main part, nano particle or the nano wire that can obtain the size homogeneous on internal layer and surface thereof are as basic structural unit.At present, the two-dimensional layered structure of people's successful use Graphene has synthesized graphene-supported metal oxide nano composite material (The Journal of Physical Chemistry Letters 2009,4,217-224; Journal of the American Chemical society, 2011,133,10878-10884).
Through the chemical reduction graphite oxide prepare Graphene be at present can the scale preparation Graphene a kind of method (Nature Nanotechnology 2009,4,217-224).But the strong reductant poisonous, that non-ambient is friendly that uses at present is the subject matter that chemical reduction prepares Graphene.The document that utilizes the photo catalytic reduction graphite oxide to prepare Graphene has had report.But the photo catalytic reduction method prepares graphene-supported tungsten oxide nano matrix material does not appear in the newspapers.
The unique two-dimensional layered structure of our comprehensive Graphenes; Advantage such as excellent chemical property and tungsten oxide nano are in each functional area application characteristic widely; Tungsten oxide nano is assembled in the Graphene material of main part as guest materials; Control synthesis condition, prepare a kind of one dimension and two-dimensional nano matrix material of uniqueness.
Summary of the invention
A kind of graphene-supported WO that the object of the present invention is to provide
3The nano wire matrix material is characterized in that one dimension and two-dimensional nano matrix material, WO
3Nanowire diameter is 10～30 nanometers, and length is 50～600 nanometers, runs through or be distributed in the internal layer or the surface of lamellar graphite alkene material of main part.
A kind of graphene-supported WO of the present invention
3The preparation method of nano wire matrix material may further comprise the steps:
(1) sodium wolframate is dissolved in the zero(ppm) water, adds acidity regulator, the concentration of regulating sodium tungstate solution is 0.1～1.0, and pH is 1.0～2.0;
(2) with step (1)) sodium tungstate solution that makes is transferred in the hydrothermal reaction kettle,, 120～200 ℃ of following hydro-thermal reactions 10～24 hours;
(3) the tungsten oxide nanometer material that step (2) is made is poured suction filtration in the vacuum filtration device into, uses deionized water wash, and vacuum-drying obtains WO in sintering between 300～500 ℃ after 2～4 hours under air atmosphere
3Nano wire.
(4) with the graphite oxide ultra-sonic dispersion in the agent of reductibility alcohol, the concentration of regulating graphite oxide is 0.5～10mg/mL, ultra-sonic dispersion 1～3 hour;
(5) WO that step (3) is made
3Nano wire mixes with the graphite oxide dispersion liquid that step (4) makes, and mixes back WO
3The mass ratio of nano wire and graphite oxide is 1: 0.01～0.5, transfers in the photo catalysis reactor, and the photo catalytic reduction reaction is 0.5～3 hour under simulated solar irradiation;
(6) pour the product of step (5) in vacuum filtration device suction filtration, use deionized water wash, obtain graphene-supported WO after the vacuum-drying
3The nano wire matrix material.
Concrete, the concentration of sodium tungstate solution can be 0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 or 1.0mol/L after the concentration adjustment;
After the acidity adjustment pH value of sodium tungstate solution can be for 1.0,1.2., 1.4,1.6,1.8 or 2.0;
Hydrothermal temperature can be 120,130,140,150,160,170,180,190 or 200 ℃; The hydro-thermal reaction time can be 10,12,14,16,18,20,22 or 24 hours;
Maturing temperature can be 300,400 or 500 ℃;
Roasting time can be 1,2,3 or 4 hour;
Graphite oxide concentration can be 0.5,1,2,3,4,5,6,7,8,9 or 10mg/mL;
Ultrasonic time can be 1,1.5,2,2.5 or 3 hour;
WO
3The mass ratio of nano wire and graphite oxide can be 1: 0.01,1: 0.05,1: 0.1,1: 0.2,1: 0.3,1: 0.4 or 1: 0.5;
The light-catalyzed reaction time can be 0.5,1.0,1.5,2,2.5 or 3 hour;
On the basis of such scheme, in the step (1), described acidity regulator is one or more the compsn in acetate, hydrochloric acid, the hydrogen peroxide;
On the basis of such scheme, in the step (4), the compsn of one or more that the pure agent of described reductibility is methyl alcohol, ethanol or terepthaloyl moietie;
On the basis of such scheme, the WO that this method is prepared
3Nano wire and graphene composite material have peacekeeping two dimension composite nanostructure, are a kind of nano composite materials.
The remarkable advantage of technical scheme of the present invention is mainly reflected in:
The reduction that the photo catalytic reduction technology is used for graphite oxide is a kind of green, environment-friendly method of reducing.Optical excitation WO when having hole trapping agents to exist
3The valence band hole that nano wire the produces agent that is hunted down is caught, and the result is under the effect of conduction band reduction potential, and graphite oxide is reduced into Graphene, simultaneously WO
3Internal layer or surface that nano wire is dispersed in Graphene form nano composite material.The advantage of this method is that the forming process of reduction and nano composite material of Graphene is easy, and reagent is cheap, helps mass preparation, for graphite oxide reduction preparation Graphene a kind of green, environment-friendly method of reducing is provided simultaneously.
Description of drawings
Fig. 1 is a kind of graphene-supported WO of the present invention
3The synoptic diagram of nano wire matrix material and preparation method thereof;
Fig. 2 is the XRD figure picture of material of main part among the embodiment 1 (Graphite Powder 99 and graphite oxide);
Fig. 3 is the XRD figure picture of product among the embodiment 1;
Fig. 4 is the SEM image of product among the embodiment 1;
Fig. 5 is the TEM image of product among the embodiment 1.
Embodiment
Embodiment one:
(1) preparation of graphite oxide.The 2g Graphite Powder 99 is joined 80 ℃ Potassium Persulphate (1g), and in the concentrated sulfuric acid solution (15mL) of Vanadium Pentoxide in FLAKES (1g), preoxidation 6 hours is cooled to room temperature afterwards, suction filtration, and washing is to neutral.The Graphite Powder 99 (2g) of preoxidation joined in 0 ℃ the 50mL concentrated sulfuric acid solution, slowly add 6g potassium permanganate afterwards, afterwards in 35 ℃ of reactions 2 hours; The ydrogen peroxide 50 that in reaction solution, slowly adds 100mL deionized water and 20mL 30% at last makes reaction terminating; Suction filtration, washing, dialysis; Make graphite oxide, its XRD figure spectrum is seen Fig. 2;
(2) WO
3The preparation of nano wire.The 3.32g sodium wolframate is joined in the 60mL zero(ppm) water, stirred 10 minutes under the room temperature, slowly drip the hydrochloric acid of 6mol/L then; Regulator solution pH is 1.5, is transferred to afterwards in the 100mL hydrothermal reaction kettle, 180 ℃ of reactions 24 hours; Suction filtration, washing was in 80 ℃ of vacuum-dryings 6 hours; Under air atmosphere, 400 ℃ of roastings 2 hours, naturally cooling obtains WO
3Nano wire.The XRD figure spectrum of product is seen Fig. 2;
(3) graphite oxide dispersion liquid preparation.With 22.5mg graphite oxide ultra-sonic dispersion in the 50mL absolute ethyl alcohol, ultrasonic time 1 hour;
(4) WO that step (2) and step (3) is obtained
3Nano wire mixes with the graphite oxide dispersion liquid, is transferred to afterwards in the photo catalysis reactor, and the photo catalytic reduction reaction is 1 hour under simulated solar irradiation, filters, and washing in 80 ℃ of vacuum-dryings 12 hours, obtains graphene-supported WO
3The nano wire nano composite material.The XRD figure spectrum of product is seen Fig. 2, and TEM figure sees Fig. 3, and SEM figure sees Fig. 4.
Embodiment two:
(1) with the step in the embodiment 1 (1);
(2) with the step in the embodiment 1 (2);
(3) graphite oxide dispersion liquid preparation.With 100mg graphite oxide ultra-sonic dispersion in the 70mL absolute ethyl alcohol, ultrasonic time 1.5 hours;
(4) WO that step (2) and step (3) is obtained
3Nano wire mixes with the graphite oxide dispersion liquid, is transferred to afterwards in the photo catalysis reactor, and the photo catalytic reduction reaction is 1.5 hours under simulated solar irradiation, filters, and washing in 80 ℃ of vacuum-dryings 12 hours, obtains graphene-supported WO
3The nano wire nano composite material.
Embodiment three:
(1) with the step in the embodiment 1 (1);
(2) with the step in the embodiment 1 (2);
(3) graphite oxide dispersion liquid preparation.With 200mg graphite oxide ultra-sonic dispersion in the 70mL absolute ethyl alcohol, ultrasonic time 1.5 hours;
(4) WO that step (2) and step (3) is obtained
3Nano wire mixes with the graphite oxide dispersion liquid, is transferred to afterwards in the photo catalysis reactor, and the photo catalytic reduction reaction is 1.5 hours under simulated solar irradiation, filters, and washing in 80 ℃ of vacuum-dryings 12 hours, obtains graphene-supported WO
3The nano wire nano composite material.
Embodiment four:
(1) with the step in the embodiment 1 (1);
(2) with the step in the embodiment 1 (2);
(3) graphite oxide dispersion liquid preparation.With 400mg graphite oxide ultra-sonic dispersion in the 70mL absolute ethyl alcohol, ultrasonic time 2 hours;
(4) WO that step (2) and step (3) is obtained
3Nano wire mixes with the graphite oxide dispersion liquid, is transferred to afterwards in the photo catalysis reactor, and the photo catalytic reduction reaction is 2 hours under simulated solar irradiation, filters, and washing in 80 ℃ of vacuum-dryings 12 hours, obtains graphene-supported WO
3The nano wire nano composite material.
Embodiment five:
(1) with the step in the embodiment 1 (1);
(2) with the step in the embodiment 1 (2);
(3) graphite oxide dispersion liquid preparation.With 600mg graphite oxide ultra-sonic dispersion in the 70mL absolute ethyl alcohol, ultrasonic time 2 hours;
(4) WO that step (2) and step (3) is obtained
3Nano wire mixes with the graphite oxide dispersion liquid, is transferred to afterwards in the photo catalysis reactor, and the photo catalytic reduction reaction is 3 hours under simulated solar irradiation, filters, and washing in 80 ℃ of vacuum-dryings 12 hours, obtains graphene-supported WO
3The nano wire nano composite material.
Embodiment six:
(1) with the step in the embodiment 1 (1);
(2) WO
3The preparation of nano wire.The 3.32g sodium wolframate is joined in the 60mL zero(ppm) water, stirred 10 minutes under the room temperature, slowly drip the hydrochloric acid of 6mol/L then; Regulator solution pH is 2, is transferred to afterwards in the 100mL hydrothermal reaction kettle, 160 ℃ of reactions 24 hours; Suction filtration, washing was in 80 ℃ of vacuum-dryings 6 hours; Under air atmosphere, 400 ℃ of roastings 2 hours, naturally cooling obtains WO
3Nano wire;
(3) with the step in the embodiment 1 (3);
(4) WO that step (2) and step (3) is obtained
3Nano wire mixes with the graphite oxide dispersion liquid, is transferred to afterwards in the photo catalysis reactor, and the photo catalytic reduction reaction is 1.5 hours under simulated solar irradiation, filters, and washing in 80 ℃ of vacuum-dryings 12 hours, obtains graphene-supported WO
3The nano wire nano composite material.
Embodiment seven:
(1) with the step in the embodiment 1 (1);
(2) WO
3The preparation of nano wire.The 3.32g sodium wolframate is joined in the 60mL zero(ppm) water, stirred 10 minutes under the room temperature, slowly drip the hydrochloric acid of 6mol/L then; Regulator solution pH is 1.5, is transferred to afterwards in the 100mL hydrothermal reaction kettle, 140 ℃ of reactions 24 hours; Suction filtration, washing was in 80 ℃ of vacuum-dryings 6 hours; Under air atmosphere, 400 ℃ of roastings 2 hours, naturally cooling obtains WO
3Nano wire;
(3) with the step in the embodiment 1 (3);
(4) WO that step (2) and step (3) is obtained
3Nano wire mixes with the graphite oxide dispersion liquid, is transferred to afterwards in the photo catalysis reactor, and the photo catalytic reduction reaction is 2 hours under simulated solar irradiation, filters, and washing in 80 ℃ of vacuum-dryings 12 hours, obtains graphene-supported WO
3The nano wire nano composite material.
Claims (6)
1. graphene-supported WO
3The nano wire matrix material is characterized in that one dimension and two-dimensional nano matrix material, WO
3Nanowire diameter is 10～100 nanometers, and length is 50～600 nanometers, runs through or be distributed in the internal layer or the surface of lamellar graphite alkene material of main part.
2. graphene-supported WO
3The preparation method of nano wire matrix material is characterized in that, this method may further comprise the steps:
(1) sodium wolframate is dissolved in the zero(ppm) water, adds acidity regulator, the concentration of regulating sodium tungstate solution is 0.1～1.0, and pH is 1.0～2.0;
(2) with step (1)) sodium tungstate solution that makes is transferred in the hydrothermal reaction kettle,, 120～200 ℃ of following hydro-thermal reactions 10～24 hours;
(3) the tungsten oxide nanometer material that step (2) is made is poured suction filtration in the vacuum filtration device into, uses deionized water wash, and vacuum-drying obtains WO in sintering between 300～500 ℃ after 2～4 hours under air atmosphere
3Nano wire.
(4) with the graphite oxide ultra-sonic dispersion in the agent of reductibility alcohol, the concentration of regulating graphite oxide is 0.5～10mg/mL, ultrasonic time is 1～3 hour;
(5) WO that step (3) is made
3Nano wire mixes with the graphite oxide dispersion liquid that step (4) makes, and mixes back WO
3The mass ratio of nano wire and graphite oxide is 1: 0.01～0.5, transfers in the photo catalysis reactor, and the photo catalytic reduction reaction is 0.5～3 hour under simulated solar irradiation;
(6) pour the product of step (5) in vacuum filtration device suction filtration, use deionized water wash, obtain graphene-supported WO after the vacuum-drying
3The nano wire matrix material.
3. a kind of graphene-supported WO according to claim 2
3The preparation method of nano wire matrix material is characterized in that: in the step (1), described acidity regulator is one or more the compsn in acetate, hydrochloric acid, the hydrogen peroxide;
4. a kind of graphene-supported WO according to claim 2
3The preparation method of nano wire matrix material is characterized in that: in the step (4), and the compsn of one or more that the pure agent of described reductibility is methyl alcohol, ethanol or terepthaloyl moietie;
5. a kind of graphene-supported WO according to claim 2
3The preparation method of nano wire matrix material, a kind of graphene-supported WO
3In the nano wire matrix material step (5), described simulated solar irradiation is an xenon lamp, and power is a kind of of 100W, 150W, 200W or 500W.
6. graphene-supported WO
3The nano wire matrix material is characterized in that: obtained by any described preparation method of claim 2-5.
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