CN107841777A - A kind of preparation method of witch culture Nano tube array of titanium dioxide - Google Patents

A kind of preparation method of witch culture Nano tube array of titanium dioxide Download PDF

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CN107841777A
CN107841777A CN201711053050.6A CN201711053050A CN107841777A CN 107841777 A CN107841777 A CN 107841777A CN 201711053050 A CN201711053050 A CN 201711053050A CN 107841777 A CN107841777 A CN 107841777A
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titanium dioxide
nano tube
tube array
electrolyte
witch culture
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CN107841777B (en
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周杰
冯波
李思杰
翁杰
鲁雄
段可
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Southwest Jiaotong University
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/26Anodisation of refractory metals or alloys based thereon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract

The invention provides a kind of preparation method of witch culture Nano tube array of titanium dioxide, belong to nano material environmental photocatlytsis technical field.1st, titanium sheet pre-processes:2nd, it is 0.8wt% ammonium fluorides mass percent to be added in 35vol% deionized water, fully dissolving, obtains ammonium fluoride solution, standby;3rd, the Disodium tungstate (Na2WO4) dihydrate that mass percent is 0.04~1wt% is added in the good ammonium fluoride solution of above-mentioned configuration, then adds the glycerine that percent by volume is 65vol%, 50 DEG C of constant temperature simultaneously stirs 30~60 minutes, obtains electrolyte;4th, pretreated titanium sheet in step 1 is connect into the positive level of power supply, graphite flake or platinized platinum connect power cathode, be placed in the electrolyte of step 3, in 30~40V constant pressure anodic oxygenization 3~5 hours, nanometer tube composite materials are obtained, are cleaned successively with ethanol and deionized water, are dried standby;5th, gained nanometer tube composite materials are placed in Muffle furnace, 450 DEG C is warming up to 5 DEG C/min of speed, and keep constant temperature 2 hours, be cooled to room temperature and obtain witch culture Nano tube array of titanium dioxide.

Description

A kind of preparation method of witch culture Nano tube array of titanium dioxide
Technical field
The invention belongs to nano material environmental photocatlytsis technical field.
Background technology
Since 1972, TiO2Photocatalysis technology decomposition water H is used by report first2And O2Afterwards, TiO2The light of semiconductor Prelude has just been pulled open in catalysis technique research.TiO2As a kind of semi-conducting material with excellent physicochemical property, in solar-electricity Pond, various sensors, body implanting material and photocatalytic pollutant degradation etc. all have broad application prospects.TiO2Nanometer Pipe array is TiO2A kind of special appearance, have that specific surface area is big, it is the advantages that immobilized performance is good, particularly suitable to be used as solar energy Battery light anode and photocatalytic pollutant degradation.Then energy gaps (anatase 3.2eV, the golden red of constrained material inherently Stone 3.0eV), TiO2It can only be excited by ultraviolet light of the wavelength less than 385nm, and to accounting for the visible light part of sunshine 95% all Efficiently it can not absorb and utilize, this have impact on TiO to a certain extent2Catalytic efficiency of the nanotube as photochemical catalyst.And Extend TiO2Spectral response range to can by light area then be improve its photocatalytic activity a kind of effective means.
W element dopings can effectively improve TiO2Photocatalytic activity because W elements doping on the one hand can be formed WO3/TiO2Heterojunction structure, suppress Carrier recombination;On the other hand, W6+With Ti4+With approximate ionic radius, can enter TiO2Intracell substitutes Ti4+Position, so as to forming new doped energy-band in forbidden band, the forbidden band for reducing composite is wide Degree so that material have can by photoresponse activity.
At present in TiO2The method that W doping is carried out in nanotube is mainly infusion process, hydro-thermal method, electro-deposition and oxide alloy Method.Although these methods can realize doping vario-property of the W elements to nanotube to a certain extent, certain lack all be present Fall into, as infusion process and electrodeposition process are difficult to control on the distributing homogeneity of W elements;Hydro-thermal method needs the operation of HTHP, Condition is harsh;The more difficult preparation of Ti-W alloys in alloy oxidation method, and the W dopings in alloy can not it is convenient regulate and control.Therefore originally Invention proposes a kind of anodizing in situ to realize W elements to TiO2The doping vario-property of nanotube, i.e., in metal Ti anodic oxygens During change forms nanotube, the W in electrolyte injects TiO simultaneously in the presence of electric field force2, so as to disposably form W TiO2 nano-tube arrays are adulterated, doping is controlled by the regulation and control to W salinity in electrolyte, are that a kind of effective doping changes Property method.
The content of the invention
It is an object of the invention to provide a kind of preparation method of witch culture Nano tube array of titanium dioxide, it can effectively be solved Certainly W elements are distributed and the controllable problem of doping in nanotube.
The purpose of the present invention is achieved through the following technical solutions:A kind of witch culture Nano tube array of titanium dioxide Preparation method, specific practice are:
Step 1: titanium sheet pre-processes:Metallic titanium surface sand paper sanding and polishing, and chemical polishing step by step, cleaning are standby;
Step 2: it is 0.8wt% fluorinations that mass percent is added in the deionized water that percent by volume is 35vol% Ammonium, stir 10 minutes, fully dissolving, obtain ammonium fluoride solution, it is standby;
Step 3: the Disodium tungstate (Na2WO4) dihydrate that mass percent is 0.04~1wt% is added into the good ammonium fluoride of above-mentioned configuration In solution, the glycerine that dissolving in 10 minutes is complete, and then addition percent by volume is 65vol% is stirred, in 50 DEG C of conditions of constant temperature Descend and stir 30~60 minutes, obtain electrolyte;
Step 4: pretreated titanium sheet in step 1 is connect into the positive level of power supply, graphite flake or platinized platinum connect power cathode, are placed in In the electrolyte of step 3, in 30~40V constant pressure anodic oxygenization 3~5 hours, nanotube sample is obtained, with ethanol and is gone Ionized water cleans successively, dries standby;
Step 5: gained nanotube sample in step 4 is placed in Muffle furnace, 450 are warming up to 5 DEG C/min of speed DEG C, and keep constant temperature 2 hours, then naturally cool to room temperature and obtain witch culture Nano tube array of titanium dioxide composite.
The mass percent of ammonium fluoride content is 0.8wt% in the electrolyte, and the mass percent of wolframic acid sodium content is 0.04~1wt%.
The electrolyte is containing 35vol%H2The binary organic system of O~65vol% glycerine.
Tungsten atom percentage composition is 0.3~1.5at% in obtained tungsten doping nano pipe array material.
The doping of wolfram element is controlled by controlling the dosage of sodium tungstate.
The invention provides a kind of preparation method of witch culture Nano tube array of titanium dioxide, due to W doping process be Anodic oxidation is carried out simultaneously during forming nanotube, W elements more uniformly spreading in whole nanotube layer.By changing The concentration of sodium tungstate in transformation electrolytic liquid, can be with the content of W elements in Effective Regulation nanotube.The W doping TiO being prepared2Receive Mitron array is perpendicular to substrate, and adhesion is good, and for nanotube caliber between 100~150nm, 4-8 μm of pipe range is adjustable, is applied to The field such as energy conversion and photocatalytic pollutant degradation.
Compared with prior art, the beneficial effects of the invention are as follows:
(1) compare and first prepare TiO at present2Nanotube introduces the preparation method of W elements by other technologies again, and the present invention is W adulterates process and TiO2The formation of nanotube is carried out simultaneously, and the constant concentration of sodium tungstate in the electrolytic solution, can ensure W members It can be uniformly distributed in element nanotube layer whole from the mouth of pipe to ttom of pipe.
(2) W doping process is only once to be formed with common titanium sheet original position anodic oxidation, without the conjunction that early stage is special Golden preparation process, without the complex process program in later stage, simplify technological process.
(3) W doping by control sodium tungstate in electrolyte concentration can it is convenient regulate and control, it is easy to operate.
Brief description of the drawings
Fig. 1 is the FE-SEM surface topography maps of the present invention
Fig. 2 is ESEM cross-section morphologies figure of the present invention
Fig. 3 is the section power spectrum Surface scan figure (a of the present invention:Surface scan corresponds to section;b:The distribution of W elements on section)
Fig. 4 is the XRD spectrum of the present invention
Embodiment
With reference to example, the invention will be further described;In described below, each reagent is that analysis is pure;To avoid Repeat, the pretreatment of titanium sheet is all unified for:Polished step by step with the SiC sand paper of 240 mesh, 400 mesh, 800 mesh, 1000 mesh and 1500 mesh Afterwards, it is cleaned by ultrasonic respectively with acetone, ethanol and deionized water, then with mixed acid solution (6.0mol/L HNO3, 1.0mol/L HF) Chemical polishing, last deionized water cleaning, drying are standby.
Embodiment one
Step 1: titanium sheet pre-processes;
It is dissolved in Step 2: weighing the ammonium fluoride (about 0.92g) that mass percent is 0.8wt% in 35mL water, stirs 10 points Clock, fully dissolve to obtain ammonium fluoride aqueous solution.
Step 3: in the ammonium fluoride aqueous solution of step 2, addition mass percent is the two of 0.04wt% (about 0.05g) Tungstic acid hydrate sodium, magnetic agitation 10 minutes, adds 65mL glycerine, magnetic agitation 30 minutes at 50 DEG C, and solution mixing is equal It is even to obtain electrolyte.
Step 4: the pretreated titanium sheet of step 1 to be connect to the positive pole of constant-voltage DC source, graphite flake or platinized platinum connect power supply Negative pole, and immerse simultaneously in the electrolyte of step 3, constant pressure 30V, electrode spacing 3cm, 25 DEG C of electrolyte constant temperature.During anodic oxidation Between be set as 3 hours, with magnetic agitation in whole process.Sample is taken out after the completion of anode oxidation process, with ethanol and gone Ionized water, which is cleaned by ultrasonic, to be dried, and obtains nanotube sample.
It is heat-treated Step 5: nanotube sample obtained by step 4 is put into temperature programmed control Muffle furnace, heating rate 5 DEG C/min.Constant temperature 2 hours after being warming up to 450 DEG C, take out sample and naturally cool to room temperature, obtain witch culture nano titania Pipe array composite material.
SEM test results show that witch culture Nano tube array of titanium dioxide is perpendicular to titanium substrate, and nanotube caliber is about 100nm, about 4 μm of pipe range, nanotube surface regular appearance.Except anatase titania and titanium substrate in XRD spectra Outside characteristic diffraction peak, the obvious characteristic diffraction peak of other materials is not observed, illustrates that wolfram element is entered with atomic level doping In the lattice of titanium dioxide.EDS and XPS results show that wolfram element is uniformly distributed in whole nanotube layer, wherein wolfram element Content about 0.3at%.
Embodiment two
Preparation process and embodiment one are essentially identical, except that:
(1) in the ammonium fluoride aqueous solution of step 2, addition mass percent is 0.08wt% (about 0.10g) two hydrations Sodium tungstate, magnetic agitation 10 minutes, adds 65mL glycerine, magnetic agitation 30 minutes at 50 DEG C, and solution is well mixed To electrolyte.
(2) the pretreated titanium sheet of step 1 is connect to the positive pole of constant-voltage DC source, graphite flake or platinized platinum connect power cathode And immerse simultaneously in electrolyte, constant pressure 35V, electrode spacing 3cm, 25 DEG C of electrolyte constant temperature.Anodizing time is set as that 3 is small When, with magnetic agitation in whole process.Sample is taken out after the completion of anode oxidation process, it is clear with ethanol and deionized water ultrasound Wash and dry, obtain nanotube sample.
(3) nanotube sample obtained by (2) is put into temperature programmed control Muffle furnace and be heat-treated, 5 DEG C/minute of heating rate Clock.Constant temperature 2 hours after being warming up to 450 DEG C, take out sample and naturally cool to room temperature, obtain witch culture Nano tube array of titanium dioxide Composite.
Test result, witch culture Nano tube array of titanium dioxide is perpendicular to titanium substrate, and nanotube caliber about 120nm is (see figure 1), about 4 μm of pipe range, nanotube surface regular appearance.Nanotube composition is mainly anatase crystal titanium dioxide, and wolfram element is with original Sub horizontal doping is entered in the lattice of titanium dioxide.Wolfram element is uniformly distributed in whole nanotube layer, wherein wolfram element Content about 0.5at%.
Embodiment three
Preparation process and embodiment one are essentially identical, except that:
(1) in the ammonium fluoride aqueous solution of step 2, addition mass percent is 0.16wt% (about 0.20g) two hydrations Sodium tungstate, magnetic agitation 10 minutes, adds 65mL glycerine, magnetic agitation 40 minutes at 50 DEG C, and solution is well mixed To electrolyte.
(2) the pretreated titanium sheet of step 1 is connect to the positive pole of constant-voltage DC source, graphite flake or platinized platinum connect power cathode And immerse simultaneously in electrolyte, constant pressure 35V, electrode spacing 3cm, 25 DEG C of electrolyte constant temperature.Anodizing time is set as that 4 is small When, with magnetic agitation in whole process.Sample is taken out after the completion of anode oxidation process, it is clear with ethanol and deionized water ultrasound Wash and dry, obtain nanotube sample.
(3) nanotube sample obtained by (2) is put into temperature programmed control Muffle furnace and be heat-treated, 5 DEG C/minute of heating rate Clock.Constant temperature 2 hours after being warming up to 450 DEG C, take out sample and naturally cool to room temperature, obtain witch culture Nano tube array of titanium dioxide Composite.
Test result, witch culture Nano tube array of titanium dioxide is perpendicular to titanium substrate, nanotube caliber about 120nm, pipe range About 6 μm (see Fig. 2), nanotube surface regular appearance.Nanotube composition is mainly anatase crystal titanium dioxide, and wolfram element is with original Sub horizontal doping is entered in the lattice of titanium dioxide.Wolfram element is uniformly distributed in whole nanotube layer, wherein wolfram element Content about 0.8at%.
Example IV
Preparation process and embodiment one are essentially identical, except that:
(1) in the ammonium fluoride aqueous solution of step 2, addition mass percent is 0.32wt% (about 0.40g) two hydrations Sodium tungstate, magnetic agitation 10 minutes, adds 65mL glycerine, magnetic agitation 50 minutes at 50 DEG C, and solution is well mixed To electrolyte.
(2) the pretreated titanium sheet of step 1 is connect to the positive pole of constant-voltage DC source, graphite flake or platinized platinum connect power cathode And immerse simultaneously in electrolyte, constant pressure 35V, electrode spacing 3cm, 25 DEG C of electrolyte constant temperature.Anodizing time is set as that 4 is small When, with magnetic agitation in whole process.Sample is taken out after the completion of anode oxidation process, it is clear with ethanol and deionized water ultrasound Wash and dry, obtain nanotube sample.
(3) nanotube sample obtained by (2) is put into temperature programmed control Muffle furnace and be heat-treated, 5 DEG C/minute of heating rate Clock.Constant temperature 2 hours after being warming up to 450 DEG C, take out sample and naturally cool to room temperature, obtain witch culture Nano tube array of titanium dioxide Composite.
Test result, witch culture Nano tube array of titanium dioxide is perpendicular to titanium substrate, nanotube caliber about 120nm, pipe range About 6 μm, nanotube surface regular appearance.Nanotube composition is mainly anatase crystal titanium dioxide, and wolfram element is with atomic level Doping is entered in the lattice of titanium dioxide.Wolfram element is uniformly distributed (see Fig. 3) in whole nanotube layer, wherein wolfram element Content about 1.0at%.
Embodiment five
Preparation process and embodiment one are essentially identical, except that:
(1) in the ammonium fluoride aqueous solution of step 2, addition mass percent is 0.64wt% (about 0.80g) two hydrations Sodium tungstate, magnetic agitation 10 minutes, adds 65mL glycerine, magnetic agitation 60 minutes at 50 DEG C, and solution is well mixed To electrolyte.
(2) the pretreated titanium sheet of step 1 is connect to the positive pole of constant-voltage DC source, graphite flake or platinized platinum connect power cathode And immerse simultaneously in electrolyte, constant pressure 40V, electrode spacing 3cm, 25 DEG C of electrolyte constant temperature.Anodizing time is set as that 5 is small When, with magnetic agitation in whole process.Sample is taken out after the completion of anode oxidation process, it is clear with ethanol and deionized water ultrasound Wash and dry, obtain nanotube sample.
(3) nanotube sample obtained by (2) is put into temperature programmed control Muffle furnace and be heat-treated, 5 DEG C/minute of heating rate Clock.Constant temperature 2 hours after being warming up to 450 DEG C, take out sample and naturally cool to room temperature, obtain witch culture Nano tube array of titanium dioxide Composite.
Test result, witch culture Nano tube array of titanium dioxide is perpendicular to titanium substrate, nanotube caliber about 150nm, pipe range About 8 μm, nanotube surface regular appearance.Nanotube composition is mainly anatase crystal titanium dioxide (see Fig. 4), and wolfram element is with original Sub horizontal doping is entered in the lattice of titanium dioxide.Wolfram element is uniformly distributed in whole nanotube layer, wherein wolfram element Content about 1.3at%.
Embodiment six
Preparation process and embodiment one are essentially identical, except that:
(1) in the ammonium fluoride aqueous solution of step 2, addition mass percent is hydrated tungsten for the two of 1.0wt% (about 1.2g) Sour sodium, magnetic agitation 10 minutes, adds 65mL glycerine, magnetic agitation 60 minutes at 50 DEG C, and solution is well mixed to be obtained Electrolyte.
(2) the pretreated titanium sheet of step 1 is connect to the positive pole of constant-voltage DC source, graphite flake or platinized platinum connect power cathode And immerse simultaneously in electrolyte, constant pressure 40V, electrode spacing 3cm, 25 DEG C of electrolyte constant temperature.Anodizing time is set as that 5 is small When, with magnetic agitation in whole process.Sample is taken out after the completion of anode oxidation process, it is clear with ethanol and deionized water ultrasound Wash and dry, obtain nanotube sample.
(3) nanotube sample obtained by (2) is put into temperature programmed control Muffle furnace and be heat-treated, 5 DEG C/minute of heating rate Clock.Constant temperature 2 hours after being warming up to 450 DEG C, take out sample and naturally cool to room temperature, obtain witch culture Nano tube array of titanium dioxide Composite.
Test result, witch culture Nano tube array of titanium dioxide is perpendicular to titanium substrate, nanotube caliber about 150nm, pipe range About 8 μm, nanotube surface regular appearance.Nanotube composition is mainly anatase crystal titanium dioxide, and wolfram element is with atomic level Doping is entered in the lattice of titanium dioxide.Wolfram element is uniformly distributed in whole nanotube layer, and wherein the content of wolfram element is about 1.5at%.

Claims (5)

1. a kind of preparation method of witch culture Nano tube array of titanium dioxide, specific practice are:
Step 1: titanium sheet pre-processes:Metallic titanium surface sand paper sanding and polishing, and chemical polishing step by step, cleaning are standby;
Step 2: it is 0.8wt% ammonium fluorides that mass percent is added in the deionized water that percent by volume is 35vol%, stir Mix 10 minutes, fully dissolving, obtain ammonium fluoride solution, it is standby;
Step 3: the Disodium tungstate (Na2WO4) dihydrate that mass percent is 0.04~1wt% is added into the good ammonium fluoride solution of above-mentioned configuration In, stir that dissolving in 10 minutes is complete, then add the glycerine that percent by volume is 65vol%, under the conditions of 50 DEG C of constant temperature simultaneously Stirring 30~60 minutes, obtains electrolyte;
Step 4: pretreated titanium sheet in step 1 is connect into the positive level of power supply, graphite flake or platinized platinum connect power cathode, are placed in step In three electrolyte, in 30~40V constant pressure anodic oxygenization 3~5 hours, nanotube sample is obtained, with ethanol and deionization Water cleans successively, dries standby;
Step 5: gained nanotube sample in step 4 is placed in Muffle furnace, 450 DEG C are warming up to 5 DEG C/min of speed, And keep constant temperature 2 hours, room temperature is then naturally cooled to, obtains witch culture Nano tube array of titanium dioxide composite.
A kind of 2. preparation method of witch culture Nano tube array of titanium dioxide according to claim 1, it is characterised in that:Institute The mass percent for stating ammonium fluoride content in electrolyte is 0.8wt%, the mass percent of wolframic acid sodium content for 0.04~ 1wt%.
A kind of 3. preparation method of witch culture Nano tube array of titanium dioxide according to claim 1, it is characterised in that:Institute It is containing 35vol%H to state electrolyte2The binary organic system of O~65vol% glycerine.
A kind of 4. preparation method of witch culture Nano tube array of titanium dioxide according to claim 1, it is characterised in that: To tungsten doping nano pipe array material in tungsten atom percentage composition be 0.3~1.5at%.
A kind of 5. preparation method of witch culture Nano tube array of titanium dioxide according to claim 1, it is characterised in that:It is logical The dosage for crossing control sodium tungstate controls the doping of wolfram element.
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CN110918088A (en) * 2019-12-27 2020-03-27 重庆市科学技术研究院 Preparation method of titanium dioxide photocatalyst
CN115814780A (en) * 2022-11-18 2023-03-21 海南大学 Preparation method of lithium-doped titanium dioxide nanowire array

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CN115814780A (en) * 2022-11-18 2023-03-21 海南大学 Preparation method of lithium-doped titanium dioxide nanowire array

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