CN102125863A - Preparation method of graphite phase carbon nitride/rutile monocrystal titanium dioxide (TiO2) nanowire array - Google Patents
Preparation method of graphite phase carbon nitride/rutile monocrystal titanium dioxide (TiO2) nanowire array Download PDFInfo
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Abstract
The invention discloses a preparation method of a graphite phase carbon nitride/rutile monocrystal titanium dioxide (TiO2) nanowire array. The preparation method is characterized by comprising the following steps: (a) dissolving a cyanamide compound or urea in a solution, immersing the prepared rutile monocrystal TiO2 nanowire array into the obtained cyanamide compound or urea solution, and then taking out and drying the nanowire array; and (b) performing heat treatment on the dried nanowire array to finally obtain the graphite phase carbon nitride/rutile monocrystal TiO2 nanowire array. The preparation method has the advantages of simple process and low cost, thus being applicable to large-scale industrial production; and the prepared graphite phase carbon nitride/rutile monocrystal TiO2 nanowire array has good visible light response activity, and can be widely applied to the fields such as photocatalysis, hydrogen production by photocatalytic decomposition of water, photoelectric conversion and the like.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide nanowire array, particularly relate to a kind of preparation method, belong to photocatalysis field with graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of visible light response activity.
Background technology
The conductor photocatalysis technology is subjected to various countries researcher's common concern owing to pure utilization pollution-free and inexhaustible solar energy can be combined with environmental protection.The single crystal titanium dioxide nanowire array that one dimension is orderly can make light induced electron directly transport along monodimension nanometer material and substrate, and minimizing photo-generated carrier (electron-hole pair) is compound crystal boundary, thereby effectively improves quantum yield (CN101786597A; Grimes, Nano Letter, 2008:3781; Eray S.Aydil, J.A.C.S, 2009:3985).But because titanium dioxide is wide band gap semiconducter body compound (3.0～3.2eV), only can utilize the ultraviolet part of sunlight irradiation (to account for about 3% of solar energy, and solar energy mainly concentrates on the visible-range of 400～800nm), solar energy utilization ratio is lower.Therefore, development has the titanium dioxide nanowire array of visible light-responded high catalytic activity for utilizing natural photodegradation environmental contaminants or photolysis water hydrogen to be significant.
At present, the existing a large amount of reports of the document of relevant titanium dioxide optical catalyst modification and patent.Wherein, by with titanium dioxide and other semi-conducting materials compound be a kind of important method of modifying.Graphite phase carbon nitride (g-C
3N
4) be a kind of novel no metal-containing polymer semiconductor light-catalyst (Wong, Nature Mater., 2009 of report recently, 8:76-80), it has the bandwidth of prohibiting less (2.7eV), spectral response range broad, unique advantages such as preparation technology is simple, and is cheap.By graphite phase carbon nitride and titanium dioxide is compound, can effectively widen spectral response range, improve photocatalysis efficiency.Prepared hud typed TiO2@ graphite phase carbon nitride composite photo-catalyst as patent CN10791565A by hydro-thermal and pyrolysis two-step reaction, the absorption sideband red shift of composite photo-catalyst is to about 475nm, under visible light irradiation, 60min is the 4-chlorophenol of degradable about 80%.Horst Kisch (Photochem.Photoblol.SCi., 2008,7,40) has also made the titanium dioxide of surfaces nitrided carbon modification by with titanium dioxide powder and urea mixed pyrolysis, and its spectral response range can extend to 750nm.But at present the report about carbonitride and titanium dioxide composite photocatalyst only is confined to nano-powder material, and it can not reduce photo-generated carrier compound at crystal boundary and catalyst particles intergranular.In addition, in concrete use, as be used for degrading organic contaminant in wastewater etc., essential through complicated photochemical catalyst separating step, also be unfavorable for adopting continuous processing that sewage is handled simultaneously.Therefore, it is cheap to explore a kind of preparation cost, and composite catalyst easy to use is significant for practical application.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, provide a kind of preparation cost cheap, easy to use, have the preparation method of good visible light-responded graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array simultaneously.
The objective of the invention is to be achieved through the following technical solutions: make carbonitride predecessor (cyanamide compound or urea) infilter light rutile single crystals titanium dioxide nanowire array by simple infusion process, the pyrolysis that heats up then can make graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array.
Graphite phase carbon nitride of the present invention/the concrete preparation process of rutile single crystals titanium dioxide nanowire array is as follows:
A) preparation rutile single crystals titanium dioxide nanowire array in substrate;
B) cyanamide compounds or urea are dissolved in the solution, again the rutile single crystals titanium dioxide nanowire array for preparing are immersed in cyanamide compounds or the urea liquid behind 1～48h, take out and dry.
C) drying is good nano-wire array is heat-treated.
Described cyanamide compounds is meant one or more mixture of cyanamide, double focusing cyanamide or melamine; The solvent of described solution can be any of distilled water or ethanol; The substrate of described rutile single crystals titanium dioxide nanowire array can be electro-conductive glass, silicon chip, titanium sheet, glass, quartz or ceramic any; Described baking temperature is 30～120 ℃; Described heat treatment temperature is 300 ℃～600 ℃, and heat treatment time is 0.5～3h, and heat-treating atmosphere is air atmosphere or natural instincts atmosphere; Described natural instincts atmosphere is meant nitrogen or argon gas.
The photolytic activity test of the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the present invention's preparation is investigated by it being assembled into Optical Electro-Chemistry (PEC) battery photolysis water hydrogen.Test process is: behind graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array welding lead, adopt epoxy sealing as working electrode, the platinum guaze conduct is to electrode, satisfy and close calomel electrode as reference electrode, 1M NaOH is as electrolyte, 300W xenon lamp (PerkinElmer) utilizes CHI 760D electrochemical workstation test photodissociation water hydrogen manufacturing performance as the simulated solar light source.From test result (Fig. 7) as can be known: applying under the condition of identical voltage, phase carbon nitride/the rutile single crystals titanium dioxide nanowire array is more unmodified much bigger as the density of photocurrent of the PEC battery of working electrode to adopt graphite, shows that the electricity conversion of photolysis water hydrogen improves.
The visible light catalysis activity test of the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the present invention's preparation is shone down by visible light, and the decolouring of methylene blue characterizes.The visible light catalysis activity test process is: with 2cm
2Array film (remainder epoxy sealing) immerses 50ml 1.25 * 10
-5The methylene blue solution of M behind the stirring 60min, is changed fresh methylene blue solution under the lucifuge, opens 300W xenon lamp (PerkinElmer) (band 420nm optical filter, the about 40mJ/cm of light intensity then
2), timing sampling is also used the absorption value of the remaining methylene blue solution of spectrophotometer (PerkinElmer Lambda 25) test at 660nm.Test result (Fig. 8) illustrates that the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the present invention's preparation has good visible light catalysis activity.
The present invention has following beneficial effect: (1) preparation technology is simple, the raw material that is adopted is the industrial chemicals of industrial-scale production and cheap, and therefore the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array cost that adopts method of the present invention to be prepared from is low.Infusion process is implemented very convenient, is fit to large-scale industrial production.Simultaneously, the present invention adopt water or cheaply ethanol both effectively reduced production cost as solvent, can not pollute simultaneously environment yet; (2) the prepared graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the present invention is very easy to use, can adopt continuous processing that sewage is handled, and can effectively reduce cost of sewage disposal; (3)) the prepared graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the present invention quantum yield height not only simultaneously also can improve solar energy utilization ratio.Because there is not crystal boundary in single crystal titanium dioxide nanowire inside, photo-generated carrier can directly transmit along nano wire and substrate, has reduced its compound at crystal boundary, thereby has improved quantum yield.In addition, the spectral response range of graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array can extend to whole visible region (850nm), has effectively improved solar energy utilization ratio.
Description of drawings
Fig. 1 is graphite phase carbon nitride of the present invention/rutile single crystals titanium dioxide nanowire array preparation process schematic diagram.
Fig. 2 is the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations and the X-ray diffractogram of Comparative Examples.
Fig. 3 is field emission scanning electron microscope (FSEM) figure of the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations.
Fig. 4 is the transmission electron microscope picture of the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations.
Fig. 5 is the high-resolution-ration transmission electric-lens figure of the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations.
Fig. 6 is the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations and the ultraviolet-visible diffuse reflection abosrption spectrogram of Comparative Examples.
Fig. 7 is the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations and the linear scan volt-ampere curve that Comparative Examples is assembled into Optical Electro-Chemistry (PEC) pond.
Fig. 8 is the performance of graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array degradation of methylene blue under visible light irradiation of the embodiment of the invention 3 preparations.
The specific embodiment
Below by specific embodiment to the invention technical scheme be further described.
The preparation of rutile single crystals titanium dioxide nanowire array can be with reference to following method, but and nonessentially is prepared in accordance with the following methods.The preparation method's of rutile single crystals titanium dioxide nanowire array change does not constitute limitation of the invention.
The preparation of rutile single crystals titanium dioxide nanowire array: under the vigorous stirring, with the titanium tetrachloride adding 400ml frozen water of 12ml, the ice-water bath cooling behind the stirring 30min, removes ice-water bath, and room temperature continues to stir 2h, makes titanium tetrachloride hydrolysis liquid.Under the room temperature, titanium tetrachloride hydrolysis liquid 24h is immersed in the substrate (electro-conductive glass, silicon chip, titanium sheet, glass, quartz or pottery etc.) that cleans up, take out and use absolute ethanol washing three times, oven dry, 550 ℃ of heating 30min promptly get dip-coating TiO then
2The substrate of crystal seed.
35ml ultra-pure water, 35ml concentrated hydrochloric acid (36～38%) are added the 100ml beaker, behind the stirring 5min, drip the 1ml tetra-n-butyl titanate, continue to stir 10min, until the solution clear.Two dip-coatings there is TiO
2100ml tetrafluoroethene liner hydrothermal reaction kettle is put in the substrate of crystal seed, and the hydrochloric acid solution with tetra-n-butyl titanate adds then, and sealed reactor after 180 ℃ of constant temperature 6h cooling room temperatures, takes out substrate, after cleaning up with ultra-pure water, and oven dry.Then, saturated solution, 35ml concentrated hydrochloric acid (36～38%) adding 100ml beaker with 27ml ultra-pure water, 8ml sodium chloride behind the stirring 5min, drip the 1ml tetra-n-butyl titanate, continue to stir 10min, until the solution clear.There is the substrate of rutile single crystals titanium dioxide nanowire array to put into 100ml tetrafluoroethene liner hydrothermal reaction kettle the preparation of last step, hydrochloric acid solution with tetra-n-butyl titanate adds then, sealed reactor, 150 ℃ of constant temperature 20h, after the cooling room temperature, substrate is taken out, after cleaning up with ultra-pure water, oven dry promptly gets the rutile single crystals titanium dioxide nanowire array.
In the present invention, adopt the FTO electro-conductive glass as a comparison case as the rutile single crystals titanium dioxide nanowire array of substrate preparation.
Embodiment 1:
With the rutile single crystals titanium dioxide nanowire array (the titanium sheet is as substrate) for preparing, behind the aqueous solution 48h of immersion 30g/L melamine, take out 120 ℃ of oven dry.Under argon atmosphere, 300 ℃ of pyrolysis 3h promptly get graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array then.
Embodiment 2:
Rutile single crystals titanium dioxide nanowire array (pottery is as substrate) with preparing behind the cyanamide aqueous solution 24h of immersion 50g/L, takes out 120 ℃ of oven dry.Under nitrogen atmosphere, 600 ℃ of pyrolysis 1h promptly get graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array then.
Embodiment 3:
With the rutile single crystals titanium dioxide nanowire array (the FTO electro-conductive glass is as substrate) for preparing, behind the ethanolic solution 12h of immersion 200g/L urea, take out 60 ℃ of oven dry.Under air atmosphere, 400 ℃ of pyrolysis 1h promptly get graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array then.
Embodiment 4:
With the rutile single crystals titanium dioxide nanowire array (simple glass is as substrate) for preparing, behind the ethanolic solution 1h of immersion 300g/L urea, take out 30 ℃ of oven dry.Under air atmosphere, 400 ℃ of pyrolysis 1h promptly get graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array then.
Embodiment 5:
With the rutile single crystals titanium dioxide nanowire array (quartz plate is as substrate) for preparing, behind the ethanolic solution 24h of immersion 100g/L urea, take out 60 ℃ of oven dry.Under air atmosphere, 500 ℃ of pyrolysis 1h promptly get graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array then.
Fig. 2 is the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations and the X-ray diffractogram of Comparative Examples.From scheming as seen, after the modification of graphite phase carbon nitride was handled, the diffraction maximum (62.8 °) of rutile 002 crystal face of the nano-wire array of embodiment preparation strengthened, and shows behind high-temperature heat treatment process, and its crystallization degree of perfection improves.
Fig. 3 is field emission scanning electron microscope (FSEM) figure of the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations.From figure as can be known: graphite phase carbon nitride/rutile single crystals titanium dioxide nano thread is evenly distributed at the FTO conductive glass surface, and is neat and orderly.
Fig. 4 is the transmission electron microscope picture of the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations.From scheming as seen: titanium dioxide nano thread directly through being about 5-10nm.
Fig. 5 is the high-resolution-ration transmission electric-lens figure of the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations.From figure as can be known, be coated with many carbonitride particles around titanium dioxide nano thread, its particle diameter is about 2nm.
Fig. 6 is the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations and the ultraviolet-visible diffuse reflection abosrption spectrogram of Comparative Examples.Show that not only there is strong absorption in graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array in the ultra-violet (UV) band, also exists stronger absorption with bright in whole visual field.
Fig. 7 is the graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array of the embodiment of the invention 3 preparations and the linear scan volt-ampere curve that Comparative Examples is assembled into Optical Electro-Chemistry (PEC) pond.From scheming as seen, when unglazed photograph, both electric currents nearly all are zero.And when illumination, along with the increase of applied voltage, density of photocurrent increases sharply, but the density of photocurrent in graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array Optical Electro-Chemistry (PEC) pond much bigger than Comparative Examples.When applied voltage was 0V (with respect to the full calomel electrode that closes), the density of photocurrent of graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array was 3.56mA/cm
2, and under the same conditions Comparative Examples only be 0.643mA/cm
2, modification is handled the back performance and has been improved about 4.5 times.
Fig. 8 is the performance of graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array degradation of methylene blue under visible light irradiation of the embodiment of the invention 3 preparations.From scheming as seen, the rutile single crystals titanium dioxide core-shell structure nano linear array of the coated with carbon bed of the present invention's preparation has high visible light response activity, 2cm
2Nano-wire array is at visible light (300W xenon lamp, PerkinElmer, band 420nm optical filter, the about 40mJ/cm of light intensity
2) under the irradiation, 120min can make 50ml 1.25 * 10
-5The methylene blue solution branch of M terminates an agreement 79%.
Claims (6)
1. the preparation method of graphite phase carbon nitride/rutile single crystals titanium dioxide nanowire array is characterized in that preparation process is as follows:
A) preparation rutile single crystals titanium dioxide nanowire array in substrate;
B) cyanamide compounds or urea are dissolved in the solution, again the rutile single crystals titanium dioxide nanowire array for preparing are immersed in cyanamide compounds or the urea liquid behind 1～48h, take out and dry.
C) drying is good nano-wire array is heat-treated.
2. according to the preparation method of the described a kind of graphite phase carbon nitride of claim 1/rutile single crystals titanium dioxide nanowire array, it is characterized in that: described cyanamide compounds is meant one or more mixture of cyanamide, double focusing cyanamide or melamine; The solvent of described solution is distilled water or ethanol.
3. according to the preparation method of the described a kind of graphite phase carbon nitride of claim 1/rutile single crystals titanium dioxide nanowire array, it is characterized in that: the substrate of described rutile single crystals titanium dioxide nanowire array is electro-conductive glass, silicon chip, titanium sheet, glass, quartz or ceramic any.
4. according to the preparation method of the described a kind of graphite phase carbon nitride of claim 1/rutile single crystals titanium dioxide nanowire array, it is characterized in that: described baking temperature is 30～120 ℃.
5. according to the preparation method of the described a kind of graphite phase carbon nitride of claim 1/rutile single crystals titanium dioxide nanowire array, it is characterized in that: described heat treatment temperature is 300 ℃～600 ℃, heat treatment time is 0.5～3h, and heat-treating atmosphere is air atmosphere or natural instincts atmosphere.
6. according to the preparation method of the described a kind of graphite phase carbon nitride of claim 6/rutile single crystals titanium dioxide nanowire array, it is characterized in that: described natural instincts atmosphere is meant nitrogen or argon gas.
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