CN107217288A - 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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- CN107217288A CN107217288A CN201710072583.2A CN201710072583A CN107217288A CN 107217288 A CN107217288 A CN 107217288A CN 201710072583 A CN201710072583 A CN 201710072583A CN 107217288 A CN107217288 A CN 107217288A
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- titania nanotube
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- deionized water
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
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- C23F3/06—Heavy metals with acidic solutions
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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 Polysorbate, 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, are widely used in sensor.
Description
Technical field
The present invention relates to titania nanotube field, more particularly to a kind of super large titania nanotube footpath regulation and control side
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 of ultrasound not only time consumption and energy consumption, and it cannot be guaranteed 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 polysorbate preferably in electrolyte.
Electrolyte fraction shared by preferably each composition is polysorbate 1%-3%, ethylene glycol 65%-67%, fluorine
Change ammonium 1%-2%, deionized water 28%-33%.
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
20 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 20
DEG C, DC voltage is 100-140V, and anodizing time is 3-5 hours.
Preferably, a kind of method in regulation and control titania nanotube footpath, the DC voltage is 140V, during anodic oxidation
Between be 4 hours.
The principle of the present invention：Pre-treatment to titanium sheet and in the electrolyte containing surfactant Polysorbate and regulate and control
Anodized and post processing are carried out under voltage, the homogeneous titania nanotube of caliber, length is obtained.Surfactant
Polysorbate is high molecular surfactant, can form Intramolecule micelle and intermolecular micella, titania nanotube is existed
Generate and reduce on micella and gather acquisition super large, homogeneous nanotube.
Beneficial effect
The present invention obtains nanotube caliber using the anodizing for adding surfactant Polysorbate in the electrolytic solution
Homogeneous with length, the titania nanotube of super large caliber, caliber can be extensive for 540nm-820nm titania nanotube
Applied to sensor.
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 20 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 polysorbate of number 1%, 1% ammonium fluoride, 65% ethylene glycol and 33% deionized water.Constant electrolyte temperature is 20
DEG C, by the logical upper 100V of two electrodes DC voltage, anodic oxidation 3 hours obtains titania nanotube.Then deionization is used
Water rinses titania nanotube 2-3 times, dries in atmosphere.The diameter of obtained nanotube is about 540nm, and length is about
3.91 μm, 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 20 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% polysorbate, 67% ethylene glycol, 1.5% ammonium fluoride and 29.5% deionized water.Constant electrolyte temperature is 20
DEG C, by the logical upper 120V of two electrodes DC voltage, anodic oxidation 5 hours obtains titania nanotube.Then deionization is used
Water rinses titania nanotube 2-3 times, dries in atmosphere.The diameter of obtained nanotube is about 650nm, and length is about
3.56 μm, nano-tube array marshalling, 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 20 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 polysorbate of number 3%, 67% ethylene glycol, 2% ammonium fluoride and 28% deionized water.Constant electrolyte temperature is 20
DEG C, by the logical upper 140V of two electrodes DC voltage, anodic oxidation 4 hours obtains titania nanotube.Then deionization is used
Water rinses titania nanotube 2-3 times, dries in atmosphere.The diameter of obtained nanotube is about 820nm, and length is about
6.10 μm, 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 polysorbate；
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 polysorbate 1%-3%, ethylene glycol 65%-67%, ammonium fluoride 1%-2%, deionized water 28%-
33%.
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 20 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 20 DEG C, and DC voltage is 100-140V, and anodizing time is 3-5 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 140V, anodizing time is 4 hours.
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| CN101037229A (en) * | 2007-04-28 | 2007-09-19 | 首都师范大学 | Preparation method of TiO2 nano material using anode alumina as template by sol-gel process |
| 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 |
| CN102070190A (en) * | 2009-11-20 | 2011-05-25 | 西南科技大学 | Ordered-structure titanium dioxide as well as preparation method and application thereof |
| CN102220616A (en) * | 2011-05-26 | 2011-10-19 | 东南大学 | Method for preparing titanium dioxide nanotube array |
| CN102502484A (en) * | 2011-09-28 | 2012-06-20 | 重庆大学 | Modified titanium dioxide nano particle nanotube and preparation method thereof |
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2017
- 2017-02-10 CN CN201710072583.2A patent/CN107217288A/en active Pending
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| CN1678514A (en) * | 2002-07-03 | 2005-10-05 | 独立行政法人科学技术振兴机构 | Noble metal nanotube and method for preparation thereof |
| CN101037229A (en) * | 2007-04-28 | 2007-09-19 | 首都师范大学 | Preparation method of TiO2 nano material using anode alumina as template by sol-gel process |
| 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 |
| CN102070190A (en) * | 2009-11-20 | 2011-05-25 | 西南科技大学 | Ordered-structure titanium dioxide as well as preparation method and application thereof |
| CN102220616A (en) * | 2011-05-26 | 2011-10-19 | 东南大学 | Method for preparing titanium dioxide nanotube array |
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Application publication date: 20170929 |