CN104087995B - A kind of preparation method of titanium dioxide nano-film - Google Patents
A kind of preparation method of titanium dioxide nano-film Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of titanium dioxide nano-film, by the device of a simple low expense, quickly prepare on various glass or silicon substrate by electric field sedimentation and produce smooth and uniform titanium dioxide nano-film.Present invention process is simple, with low cost, equipment needed thereby simple, and treatment conditions are gentle, and gained film uniformity is good.
Description
Technical field
The present invention relates to preparation method of nano material technical field, the preparation method of a kind of titanium dioxide nano-film.
Background technology
Nano titanium oxide is the semi-conducting material of a kind of broad stopband width, has the optics of excellence, electricity and chemical stability chemical property, has been widely used in quasiconductor, sensor, dielectric material, coating and catalyst field.But the use of its superior optics, electricity and magnetic property is mainly with the form of titanium deoxid film.The titanium dioxide surface of raying can occur the photocatalysis of titanium dioxide. and there is the shortcoming such as easy in inactivation, difficult recovery in powder photocatalyst titanium dioxide so that it is and application is restricted.In addition to solar energy is changed, under the irradiation of ultraviolet light, titanium deoxid film also has the function purifying the novelties such as air, sterilization, deodorization, Superhydrophilic.And can catalyzing and synthesizing, noble metal recovery, the field such as waste water process find application.Thus be the novel capabilities material of a class great potential, can be applied at industrial circle widely.
At present, prepare titanium deoxid film method and still suffer from some problems.The physical preparation method of titanium deoxid film includes reaction magnetocontrol sputtering, electron beam evaporation, ion beam assisted depositing etc., and compared to preparing the chemical gaseous phase depositing process of thin film, required substrate temperature is relatively low, is difficult to cause the deformation of matrix and cracking.But become the method for phase easily to generate impurity phase after its first film forming, but also need accurate state modulator.The same with chemical gaseous phase depositing process, physics preparation needs vacuum system, and Preparation equipment is expensive.And the liquid phase preparation process without the titanium deoxid film of special expensive equipment has various various.But the raw material used by the predecessor of sol-gel process is generally the alkoxide of expensive titaniferous, and gel preparation needs substantial amounts of organic solvent, and cost is bigger, and thin film and the poor adhesive force of matrix, thin film is easily cracked in dry run subsequently.The film layer structure ratio utilizing the hydrolysis-sedimentation method to prepare titanium dioxide film prepared is more uniform, and adhesive force is relatively good, but in preparation process, reaction condition is needed strict control.Titanium salt needed for the preparation of solution simultaneously, such as TiCl4, or toxicity is bigger.Although liquid phase deposition is not required to the equipment of costliness. simple to operate, but it is to utilize the chemical equilibrium reaction between the titanium ion of fluorine in aqueous solution and titanium dioxide, introducing network in the solution and effect in conjunction with boric acid, by titanium dioxide deposition to being immersed on the carrier in reactant liquor, but preparation process holding time is oversize, and the metal coordination ion of fluorine may be to environmental effects.
Summary of the invention
It is an object of the invention to for above-mentioned deficiency of the prior art, it is provided that a kind of method preparing titanium dioxide nano-film by simple electric field deposition method.
The present invention is that the nano TiO 2 powder purchased with business is as raw material, device by a simple low expense, open deposition circuit is used to carry out currentless electrostatic precipitation, add with minor compound, on various glass or silicon substrate, quickly preparation produces smooth and uniform titanium dioxide nano-film, to solve preparing, at sol-gel process, sputtering method and liquid phase deposition etc., the problems referred to above that titanium dioxide nano-film is occurred.
In electrochemical deposition method, the base material of usual thin film to be deposited doubles as an electrode, with power supply, other electrode and one closed path loop of deposition liquid composition.Under electric field action, while in dispersion liquid, the generation directed movement of microgranule and ion and electrode reaction form thin film, the electrode reaction that some of such as bubble or chemical reaction are harmful, deposition process and deposition film quality can be adversely affected.
It is an object of the invention to be achieved through the following technical solutions:
The preparation method of a kind of titanium dioxide nano-film, this preparation method comprises the steps:
(1) preparation dispersed deposition liquid
The nano titanium dioxide powder that active surface agent and particle diameter are 10 50nm is added in deionized water and prepares dispersed deposition liquid, described active surface agent is rare earth nitrate, wherein, the molar concentration of nano titanium oxide is 0.005 0.02mol/L, the molar concentration of active surface agent is 0.02 0.05 times of nano titanium oxide molar concentration, and molar concentration is about 0.0002 0.001mol/L, after ultrasound wave is sufficiently stirred for 30 minutes, stand 12 hours, stand-by；
(2) electric field deposition
The dispersed deposition liquid that step (1) is prepared is joined and is provided with outside two in the glass container of depositing electrode, the glass cleaned scrubbing and surface activation process crossed or silicon chip are placed in dispersed deposition liquid as deposition substrate and carry out electric field deposition, deposition voltage is 6000 30000V, electrodeposition time is 10 minutes 90 minutes, electrode spacing 20mm 50mm, through electric field deposition, deposition substrate forms titanium deoxid film.
(3) annealing
Putting in muffle furnace after the thin film nature airing that step (2) prepares and be progressively heated at 300-500 DEG C with the speed of 20 DEG C/min, temperature retention time is furnace cooling after 1 hour.
Further in scheme, the method cleaning scrubbing and surface activation process described in step (2) is: after deionized water rinsing deposition substrate 23 times, deposition substrate is immersed respectively use ultrasonic waves for cleaning 20 minutes in acetone and ethanol, then deposition substrate taking-up is put into use ultrasonic waves for cleaning 10 minutes in deionized water.Before use, immerse in 2M dilute hydrochloric acid solution in activation 5 minutes, finally rinse well with deionized water.
Further in scheme, described active surface agent is the nitrate of ytterbium, lanthanum or neodymium.
Further in preferred version, in step (1), the particle diameter of nano titanium dioxide powder is 15 40nm.
Further in preferred version, in step (1), the molar concentration of nano titanium oxide is 0.006 0.015mol/L.
Further in preferred version, in step (1), the molar concentration of active surface agent is 0.00025 0.0008mol/L.
Further in preferred version, in step (2), electric field deposition deposition voltage is 8000 25000V, electrode spacing 20mm 30mm.
The present invention has a beneficial effect highlighted below:
1, technique is simple, with low cost, equipment needed thereby is simple, and treatment conditions are gentle, it is to avoid the phase counterdiffusion of thin film and sixbstrate components before and after processing, gained thin film purity height, homogeneity is good.
2, no current in deposition circuit, it is to avoid chemical reaction on depositing electrode, or bubble produce the impact that thin film is formed quality；Easily preparing certain thickness smooth and uniform nano thin-film as on the glass of deposition substrate or silica-based, avoiding poisonous additive and gas in Conventional electrochemical deposition process simultaneously and discharge environmental pollution.
3, directly use the nano-metal-oxide raw material that business is purchased, the preparation of dispersed deposition liquid is simple, it is to avoid the raw material that traditional electrolyte is complicated adds and preparation process.
4, in liquid phase prepares, organic alkoxide etc. is not used, it is to avoid song, cracking, grain coarsening, thin film and the defect such as substrate or atmosphere reaction that thin film may cause in subsequent processes.
5, active rare-earth surface agent substantially accelerates efficiency or the speed of electric field deposition nanophase titania films, and makes the Quality advance of institute's deposition of titania nano thin-film.
Accompanying drawing explanation
Fig. 1 is the electric field deposition device schematic diagram of the titanium dioxide nano-particle deposition of the present invention；
In figure, 1-glass container, 2-dispersed deposition liquid, 3-depositing electrode, 4-deposition substrate, 5-plus high-pressure power supply；
Fig. 2 is the SEM image of the smooth sheet glass basal plane as deposition substrate to be deposited；
Fig. 3 is the SEM image of the titanium dioxide nano-film prepared in embodiment 1；
Fig. 4 is the SEM image of the titanium dioxide nano-film prepared in embodiment 2.
Fig. 5 is the SEM image of the titanium dioxide nano-film prepared in embodiment 3；
Fig. 6 is the SEM image of the titanium dioxide nano-film prepared in embodiment 4.
Fig. 7 is the SEM image of the titanium dioxide nano-film prepared in embodiment 5；
Detailed description of the invention
Below in conjunction with the accompanying drawings and embodiment the invention will be further described:
The schematic diagram of electric field deposition device used in example 1 below-4 sees Fig. 1, the aluminium sheet that the is parallel to each other depositing electrode 3 as electric field deposition is placed in glass container 1 both sides, depositing electrode 3 is connected with plus high-pressure power supply, plus forming highfield between depositing electrode after high voltage 3, make the nano titanium oxide displacement being dispersed in dispersed deposition liquid 2, it is deposited on the glass as deposition substrate 4 or silicon chip, is formed on corresponding titanium deoxid film.
Embodiment
1
:
0.0125mol nanometer titanium dioxide titanium valve (particle diameter 25 nanometer) and 2.6*10 is added at 1000ml deionized water-4Mol active surface agent Y (NO3)3•6H2O.Under JY92-II supersonic cell disintegrating machine with 30 DEG C, 2% intensity, interval 5 seconds stir 30 minutes, formed titanium dioxide dispersed deposition liquid.For electric field deposition after standing 12 hours.
After deionized water rinsing deposition substrate 2 times, deposition substrate 4 is immersed respectively use ultrasonic waves for cleaning 20 minutes in acetone and ethanol, then deposition substrate 4 taking-up is put into use ultrasonic waves for cleaning 10 minutes in deionized water.Immerse before use in 2M dilute hydrochloric acid 5 minutes.Then, filling by the glass container in titanium dioxide dispersed deposition liquid electric field deposition device prepared above shown in Fig. 1 is put into.50mm between aluminum plate electrodes, control deposition voltage is 25kv, carries out electric field deposition 20 min, promotes the nano-titanium oxide displacement being dispersed in dispersed deposition liquid 3, formation of deposits titanium deoxid film in deposition substrate 4.
Then put in muffle furnace after the thin film nature airing prepared by electro-deposition and be progressively heated at 500 DEG C with the speed of 20 DEG C/min, temperature retention time 1h, subsequently furnace cooling.
Fig. 2 show the SEM image of the smooth sheet glass basal plane as deposition substrate 4 to be deposited, Fig. 3 is the SEM image of the titanium dioxide nano-film in the deposition substrate that the preparation technology in embodiment 1 prepares, the tissue topography of titanium dioxide nano-film can be observed, thin film smooth even, film does not observes obvious hole and crackle.
Embodiment
2
:
0.0125mol nanometer titanium dioxide titanium valve (particle diameter 40 nanometer) and 2.6*10 is added at 1000ml deionized water-4Mol active surface agent Y (NO3)3•6H2O.Under JY92-II supersonic cell disintegrating machine with 30 DEG C, 2% intensity, interval 5 seconds stir 30 minutes, formed titanium dioxide dispersed deposition liquid.For electric field deposition after standing 12 hours.
After deionized water rinsing deposition substrate 3 times, deposition substrate 4 is immersed respectively use ultrasonic waves for cleaning 20 minutes in acetone and ethanol, then deposition substrate 4 taking-up is put into use ultrasonic waves for cleaning 10 minutes in deionized water.Immerse before use in 2M dilute hydrochloric acid 5 minutes.Then, filling by the glass container in titanium dioxide dispersed deposition liquid electric field deposition device prepared above shown in Fig. 1 is put into.30mm between aluminum plate electrodes, control deposition voltage is 20kv, carries out electric field deposition 10 min, promotes the nano-titanium oxide displacement being dispersed in dispersed deposition liquid 3, formation of deposits titanium deoxid film in deposition substrate 4.
Then put in muffle furnace after the thin film nature airing prepared by electro-deposition and be progressively heated at 500 DEG C with the speed of 20 DEG C/min, temperature retention time 1h, subsequently furnace cooling.Fig. 4 is the SEM image of the titanium dioxide nano-film in the deposition substrate that the preparation technology in embodiment 2 prepares, and can observe the tissue topography of titanium dioxide nano-film, dispersed the titania nanoparticles of size uniform in thin film.
Embodiment
3
:
0.0125mol nanometer titanium dioxide titanium valve (particle diameter 20 nanometer) and 5.8*10 is added at 1000ml deionized water-4Mol active surface agent Y (NO3)3•6H2O.Under JY92-II supersonic cell disintegrating machine with 30 DEG C, 2% intensity, interval 5 seconds stir 10 minutes, formed titanium dioxide dispersed deposition liquid.For electric field deposition after standing 12 hours.
After deionized water rinsing deposition substrate 3 times, deposition substrate 4 is immersed respectively use ultrasonic waves for cleaning 20 minutes in acetone and ethanol, then deposition substrate 4 taking-up is put into use ultrasonic waves for cleaning 10 minutes in deionized water.Immerse before use in 2M dilute hydrochloric acid 5 minutes.Then, filling by the glass container in titanium dioxide dispersed deposition liquid electric field deposition device prepared above shown in Fig. 1 is put into.25mm between aluminum plate electrodes, control deposition voltage is 8kv, carries out electric field deposition 40 min, promotes the nano-titanium oxide displacement being dispersed in dispersed deposition liquid 3, formation of deposits titanium deoxid film in deposition substrate 4.Then, after the thin film nature airing prepared by electro-deposition, put in muffle furnace and be progressively heated at 500 DEG C with the speed of 20 DEG C/min, temperature retention time 1h, subsequently furnace cooling.Fig. 5 is the SEM image of the titanium dioxide nano-film in the deposition substrate that the preparation technology in embodiment 3 prepares, and can observe the tissue topography of titanium dioxide nano-film, titania nanoparticles distribution uniform in thin film, and particle size is the most tiny.
Embodiment
4
:
0.0075mol nanometer titanium dioxide titanium valve (particle diameter 25 nanometer) and 2.2*10 is added at 1000ml deionized water-4Mol active surface agent Y (NO3)3•6H2O.Under JY92-II supersonic cell disintegrating machine with 30 DEG C, 2% intensity, interval 5 seconds stir 30 minutes, formed titanium dioxide dispersed deposition liquid.For electric field deposition after standing 12 hours.
After deionized water rinsing deposition substrate 2 times, deposition substrate 4 is immersed respectively use ultrasonic waves for cleaning 20 minutes in acetone and ethanol, then deposition substrate 4 taking-up is put into use ultrasonic waves for cleaning 10 minutes in deionized water.Immerse before use in 2M dilute hydrochloric acid 5 minutes.Then, filling by the glass container in titanium dioxide dispersed deposition liquid electric field deposition device prepared above shown in Fig. 1 is put into.35mm between aluminum plate electrodes, control deposition voltage is 15kv, carries out electric field deposition 50 min, promotes the nano-titanium oxide displacement being dispersed in dispersed deposition liquid 3, formation of deposits titanium deoxid film in deposition substrate 4.
Then put in muffle furnace after the thin film nature airing prepared by electro-deposition and be progressively heated at 500 DEG C with the speed of 20 DEG C/min, temperature retention time 1h, subsequently furnace cooling.Fig. 6 is the SEM image of the titanium dioxide nano-film in the deposition substrate that the preparation technology in embodiment 3 prepares, and can observe the tissue topography of titanium dioxide nano-film, thin film smooth even, and intramembranous particles distributing homogeneity is good.
Embodiment
5
:
0.01mol nanometer titanium dioxide titanium valve (particle diameter 25 nanometer) and 2.6*10 is added at 1000ml deionized water-4Mol active surface agent La (NO3)3•6H2O.Under JY92-II supersonic cell disintegrating machine with 30 DEG C, 2% intensity, interval 5 seconds stir 30 minutes, formed titanium dioxide dispersed deposition liquid.For electric field deposition after standing 12 hours.
After deionized water rinsing deposition substrate 3 times, deposition substrate 4 is immersed respectively use ultrasonic waves for cleaning 20 minutes in acetone and ethanol, then deposition substrate 4 taking-up is put into use ultrasonic waves for cleaning 10 minutes in deionized water.Immerse before use in 2M dilute hydrochloric acid 5 minutes.Then, filling by the glass container in titanium dioxide dispersed deposition liquid electric field deposition device prepared above shown in Fig. 1 is put into.40mm between aluminum plate electrodes, control deposition voltage is 15kv, carries out electric field deposition 30 min, promotes the nano-titanium oxide displacement being dispersed in dispersed deposition liquid 3, formation of deposits titanium deoxid film in deposition substrate 4.
Then put in muffle furnace after the thin film nature airing prepared by electro-deposition and be progressively heated at 500 DEG C with the speed of 20 DEG C/min, temperature retention time 1h, subsequently furnace cooling.Fig. 7 is the SEM image of the titanium dioxide nano-film in the deposition substrate that the preparation technology in embodiment 5 prepares, and uses active surface agent Y (NO with precedent3)3•6H2The various sedimentary conditions of O compare, and can observe titanium dioxide nano-film still smooth even, and intramembranous particles is evenly distributed.
AboveEmbodiment 1-5It it is presently preferred embodiments of the present invention; the present invention should not be limited to the above-mentioned each embodiment refered in particular to; and those skilled in the art can derive many improvement and change. all changes made according to technical solution of the present invention; when produced function is without departing from the scope of technical solution of the present invention, belong to protection scope of the present invention.
Claims (6)
1. the preparation method of a titanium dioxide nano-film, it is characterised in that this preparation method comprises the steps:
(1) preparation dispersed deposition liquid
The nano titanium dioxide powder that active surface agent and particle diameter are 10 50nm is added in deionized water and prepares dispersed deposition liquid, described active surface agent is rare earth nitrate, wherein, the molar concentration of nano titanium oxide is 0.005 0.02mol/L, the molar concentration of active surface agent is 0.0002 0.001mol/L, after ultrasound wave is sufficiently stirred for 30 minutes, stand 12 hours, stand-by；
(2) electric field deposition
The dispersed deposition liquid that step (1) is prepared joins outside be provided with in the glass container of a pair depositing electrode, the glass cleaned scrubbing and surface activation process crossed or silicon chip are placed in dispersed deposition liquid as deposition substrate and carry out electric field deposition, deposition voltage is 6000 30000V, electrodeposition time is 10 minutes 90 minutes, electrode spacing 20mm 50mm, through electric field deposition, deposition substrate forms titanium deoxid film；
(3) annealing
Putting in muffle furnace after the thin film nature airing that step (2) prepares and be progressively heated at 300-500 DEG C with the speed of 20 DEG C/min, temperature retention time is furnace cooling after 1 hour.
The preparation method of titanium dioxide nano-film the most according to claim 1, it is characterized in that, the method cleaning scrubbing and surface activation process described in step (2) is: after deionized water rinsing deposition substrate 23 times, deposition substrate is immersed respectively use ultrasonic waves for cleaning 20 minutes in acetone and ethanol, then deposition substrate taking-up is put into use ultrasonic waves for cleaning 10 minutes in deionized water；Before carrying out step (2) electric field deposition, immerse in 2M dilute hydrochloric acid solution in activation 5 minutes, finally rinse well with deionized water.
The preparation method of titanium dioxide nano-film the most according to claim 1, it is characterised in that described active surface agent is the nitrate of ytterbium, lanthanum or neodymium.
The preparation method of titanium dioxide nano-film the most according to claim 1, it is characterised in that in step (1), the molar concentration of active surface agent is 0.00025 0.0008mol/L.
The preparation method of titanium dioxide nano-film the most according to claim 1, it is characterised in that in step (1), the molar concentration of nano titanium oxide is 0.006 0.015mol/L, the particle diameter of nano titanium dioxide powder is 15 40nm.
The preparation method of titanium dioxide nano-film the most according to claim 1, it is characterised in that in step (2), electric field deposition deposition voltage is 8000 25000V, electrode spacing 20mm 30mm.
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