CN107217287A - A kind of method in regulation and control titania nanotube footpath - Google Patents
A kind of method in regulation and control titania nanotube footpath Download PDFInfo
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- CN107217287A CN107217287A CN201710072574.3A CN201710072574A CN107217287A CN 107217287 A CN107217287 A CN 107217287A CN 201710072574 A CN201710072574 A CN 201710072574A CN 107217287 A CN107217287 A CN 107217287A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a kind of method in regulation and control titania nanotube footpath.Titanium sheet is subjected to chemical polishing in hydrofluoric acid and salpeter solution；On the constant temperature anodic oxidation device that titanium sheet after polishing is positioned over to two electrodes, titanium sheet after polishing is used as anode, graphite electrode is negative electrode, two electrodes is immersed in same electrolyte, electrolyte is made up of surfactant sodium dodecyl base benzene sulfonic acid sodium salt, ethylene glycol, ammonium fluoride and deionized water；Electrolyte temperature is set, by the logical upper DC voltage of two electrodes, anodic oxidation is carried out, obtains titania nanotube；Titania nanotube is rinsed 23 times with deionized water, dried in atmosphere.The titania nanotube caliber obtained is up to hundreds of nanometers, and nano-tube array is regular, and caliber and length are homogeneous, can be applied to solar cell.
Description
Technical field
The present invention relates to a kind of method in regulation and control titania nanotube footpath, more particularly to a kind of super large nano titania
Caliber regulates and controls method.
Background technology
Titania nanotube has bigger serface and excellent photoelectric properties, in DSSC, life
The fields such as thing sensing, biological medicine, hydrogen sensor, catalyst carrier are with a wide range of applications.Titania nanotube
Preparation method mainly has sol-gel process, template, high temperature hydro-thermal method and anodizing.Wherein, anodizing technique letter
Single, controllability is good, therefore enjoys and pay close attention to both at home and abroad.Generally, anodizing mainly takes electrolyte to be aoxidized, electrolysis
Liquid solute is mainly fluoride, and solvent is alcohols material.Using an anodizing, it can be formed in the open top end of nanotube
One layer of unordered impurity and the nanotube of lodging, have blocked the opening of array, have generally had large effect to practical application.It is existing
There are many technologies to take Two-step anodization to obtain the titania nanotube that pattern is more regular.CN201110138088.X,
The preparation method for the Nano tube array of titanium dioxide that Southeast China University proposes prepares nanotube with two-step electrochemical anodizing method, but wherein
The step time consumption and energy consumption of ultrasound, and do not ensure that nanotube prepared by all once oxidations is all shaken off.
Surfactant has prepared the additive of the nano materials such as nanometer rods, nanotube as soft template,
The cationic surfactant auxiliary that CN201310177283.2 Harbin Engineering Universitys propose prepares titania nanotube
Method utilizes soft template-hydro-thermal method that surfactant is used for the preparation of titania nanotube powder, obtains more uniform, into
The high caliber of tube efficiency.
Titanium dioxide caliber increases, and is conducive to improving the light hydrolysis property of titania nanotube.In anodizing,
The titania nanotube for preparing super large caliber using titanium sheet has no relevant report.
The content of the invention
The purpose of the present invention is that acquisition nanotube caliber and length are homogeneous, the titania nanotube of super large caliber.
The technical solution adopted for the present invention to solve the technical problems is：A kind of side in regulation and control titania nanotube footpath
Method, it is characterised in that concretely comprise the following steps：
A. titanium sheet is subjected to chemical polishing in acid solution；
B. electrolyte quota：Electrolyte is made up of surfactant, ethylene glycol, ammonium fluoride and deionized water；
C. the titanium sheet after polishing is positioned on the constant temperature anodic oxidation device of two electrodes, the titanium sheet conduct after polishing
Anode, graphite electrode is negative electrode, and two electrodes are immersed in same electrolyte；
D., electrolyte temperature is set, by the logical upper DC voltage of two electrodes, anodic oxidation is carried out, obtains nano titania
Pipe；
E. titania nanotube is rinsed 2-3 times with deionized water, dried in atmosphere.
Surfactant is neopelex preferably in electrolyte.
Electrolyte fraction shared by preferably each composition is neopelex 1%-5%, ethylene glycol 48%-
50%, ammonium fluoride 1%-2%, deionized water 43%-50%.
A kind of method in described regulation and control titania nanotube footpath, it is characterised in that：The titanium sheet purity>99%, it is thick
Spend for 1-3mm.
A kind of method in described regulation and control titania nanotube footpath, it is characterised in that：The described chemical polishing time is
15 seconds.
A kind of method in described regulation and control titania nanotube footpath, it is characterised in that：The acid solution is by hydrofluoric acid, nitre
Acid and deionized water composition, hydrofluoric acid, nitric acid, the volume ratio of deionized water are 1：1：2.
A kind of method in described regulation and control titania nanotube footpath, it is characterised in that：Described electrolyte temperature is 10
DEG C, DC voltage is 50-80V, and anodizing time is 2-3 hours.
Preferably, a kind of method in regulation and control titania nanotube footpath, the DC voltage is 60V, during anodic oxidation
Between be 3 hours.
The principle of the present invention：Pre-treatment to titanium sheet and in the electrolyte containing surfactant sodium dodecyl base benzene sulfonic acid sodium salt
Neutralize and carry out anodized and post processing under regulation and control voltage, obtain the homogeneous titania nanotube of caliber, length.Table
Face activating agent neopelex is aqueous anion surfactant, can form micella, make titania nanotube
Generate and reduce on micella and gather acquisition super large, homogeneous nanotube.
Beneficial effect
The present invention is received using the anodizing for adding surfactant sodium dodecyl base benzene sulfonic acid sodium salt in the electrolytic solution
Mitron caliber and length are homogeneous, the titania nanotube of super large caliber, and caliber is 450-750nm titania nanotube energy
It is enough to be more preferably applied to solar cell.
Brief description of the drawings
Titania nanotube footpath FETEM (field emission scanning electron microscope) figure that Fig. 1 embodiments 1 are obtained；
Titania nanotube footpath FETEM (field emission scanning electron microscope) figure that Fig. 2 embodiments 2 are obtained；
Titania nanotube footpath FETEM (field emission scanning electron microscope) figure that Fig. 3 embodiments 3 are obtained.
Embodiment
With reference to embodiment, the present invention is expanded on further.
Embodiment 1：
It is that the titanium sheet that 99.9%, thickness is 1mm in the volume ratio of hydrofluoric acid, nitric acid and deionized water is 1 by purity：1：2
Acid solution in chemical polishing 15 seconds.On the anodic oxidation device that titanium sheet after polishing is positioned over to two electrodes, after polishing
Titanium sheet as anode, graphite electrode is negative electrode；Two electrodes are immersed in same electrolyte.The composition of electrolyte is volume integral
The neopelex of number 1%, 1% ammonium fluoride, 50% ethylene glycol and 48% deionized water.Electrolyte temperature is permanent
It is set to 10 DEG C, by the logical upper 50V of two electrodes DC voltage, anodic oxidation 2 hours obtains titania nanotube.Then use
Deionized water rinses titania nanotube 2-3 times, dries in atmosphere.The diameter of obtained nanotube is about 450nm, long
About 1.92 μm of degree, nano-tube array marshalling, length is consistent, uniform diameter.
Embodiment 2：
It is that the titanium sheet that 99.9% thickness is 2mm in the volume ratio of hydrofluoric acid, nitric acid and deionized water is 1 by purity：1：2
Chemical polishing 15 seconds in acid solution.On the anodic oxidation device that titanium sheet after polishing is positioned over to two electrodes, after polishing
Titanium sheet is as anode, and graphite electrode is negative electrode；Two electrodes are immersed in same electrolyte.The composition of electrolyte is volume fraction
2.5% neopelex, 50% ethylene glycol, 1.5% ammonium fluoride and 46% deionized water.Electrolyte temperature
Constant is 10 DEG C, and by the logical upper 60V of two electrodes DC voltage, anodic oxidation 3 hours obtains titania nanotube.Then
Titania nanotube is rinsed 2-3 times with deionized water, dried in atmosphere.The diameter of obtained nanotube is about 610nm,
Length is about 2.96 μm, nano-tube array marshalling, and length is consistent, uniform diameter.
Embodiment 3：
It is 99.9% by purity, the titanium sheet that thickness is 3mm is 1 in the volume ratio of hydrofluoric acid, nitric acid and deionized water：1：2
Acid solution in chemical polishing 15 seconds.On the anodic oxidation device that titanium sheet after polishing is positioned over to two electrodes, after polishing
Titanium sheet as anode, graphite electrode is negative electrode；Two electrodes are immersed in same electrolyte.The composition of electrolyte is volume integral
The neopelex of number 5%, 48% ethylene glycol, 2% ammonium fluoride and 45% deionized water.Electrolyte temperature is permanent
It is set to 10 DEG C, by the logical upper 80V of two electrodes DC voltage, anodic oxidation 2 hours obtains titania nanotube.Then use
Deionized water rinses titania nanotube 2-3 times, dries in atmosphere.The diameter of obtained nanotube is about 750nm, long
About 1.68 μm of degree, nano-tube array marshalling, length is consistent, uniform diameter.
It should be understood that these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it is to be understood that
After the content of the invention lectured has been read, those skilled in the art can make various changes or modifications to the present invention, these
The equivalent form of value equally falls within the application appended claims limited range.
Claims (7)
1. a kind of method in regulation and control titania nanotube footpath, it is characterised in that concretely comprise the following steps：
A. titanium sheet is subjected to chemical polishing in acid solution；
B. electrolyte quota：Electrolyte is made up of surfactant, ethylene glycol, ammonium fluoride and deionized water, and described surface is lived
Property agent be neopelex；
C. the titanium sheet after polishing is positioned on the constant temperature anodic oxidation device of two electrodes, the titanium sheet after polishing is used as sun
Pole, graphite electrode is negative electrode, and two electrodes are immersed in same electrolyte；
D., electrolyte temperature is set, by the logical upper DC voltage of two electrodes, anodic oxidation is carried out, obtains titania nanotube；
E. titania nanotube is rinsed 2-3 times with deionized water, dried in atmosphere.
2. a kind of method in regulation and control titania nanotube footpath according to claim 1, it is characterised in that：Shared by each composition
Electrolyte fraction is neopelex 1%-5%, ethylene glycol 48%-50%, ammonium fluoride 1%-2%, deionization
Water 43%-50%.
3. a kind of method in regulation and control titania nanotube footpath according to claim 1, it is characterised in that：The titanium sheet is pure
Degree>99%, thickness is 1-3mm.
4. a kind of method in regulation and control titania nanotube footpath according to claim 1, it is characterised in that：Described chemistry
Polishing time is 15 seconds.
5. a kind of method in regulation and control titania nanotube footpath according to claim 1, it is characterised in that：The acid solution
It is made up of hydrofluoric acid, nitric acid and deionized water, hydrofluoric acid, nitric acid, the volume ratio of deionized water are 1：1：2.
6. a kind of method in regulation and control titania nanotube footpath according to claim 1, it is characterised in that：Described electrolysis
Liquid temperature degree is 10 DEG C, and DC voltage is 50-80V, and anodizing time is 2-3 hours.
7. a kind of method in regulation and control titania nanotube footpath according to claim 1, it is characterised in that：The direct current
Press as 60V, anodizing time is 3 hours.
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| CN103074661A (en) * | 2013-01-07 | 2013-05-01 | 南昌航空大学 | Method for controlling hydrophily and hydrophobicity of array surface of titanium dioxide nanotube |
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| CN105271175A (en) * | 2015-11-16 | 2016-01-27 | 中南大学 | Dispersion method of carbon nano tube |
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2017
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| CN101104953A (en) * | 2007-04-28 | 2008-01-16 | 首都师范大学 | Method for preparing TiO2 nano material by direct current deposition method using anode aluminum oxide as template |
| CN101608333A (en) * | 2008-06-16 | 2009-12-23 | 吴昊 | Titanium alloy electrochemical oxidation liquid |
| CN101785880A (en) * | 2009-12-31 | 2010-07-28 | 东南大学 | Blood vessel bracket utilizing titanium oxide nanotube to load medicine |
| CN102127779A (en) * | 2010-12-25 | 2011-07-20 | 太原理工大学 | Method for preparing copper oxide nano tube |
| CN102220616A (en) * | 2011-05-26 | 2011-10-19 | 东南大学 | Method for preparing titanium dioxide nanotube array |
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