CN102115903B - Method for preparing titanium dioxide nano-ring through anodic oxidation - Google Patents
Method for preparing titanium dioxide nano-ring through anodic oxidation Download PDFInfo
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- CN102115903B CN102115903B CN2011100242755A CN201110024275A CN102115903B CN 102115903 B CN102115903 B CN 102115903B CN 2011100242755 A CN2011100242755 A CN 2011100242755A CN 201110024275 A CN201110024275 A CN 201110024275A CN 102115903 B CN102115903 B CN 102115903B
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Abstract
The invention belongs to the technical field of preparing nanophase materials as well as the field of optoelectronic information materials, and particularly relates to a method for preparing a titanium dioxide nano-ring by adopting anodic oxidation. The method comprises the following steps of: using a titanium sheet as a raw material, carrying out pretreatment of deoiling, cleaning, and the like on the raw material, adopting the pretreated titanium sheet as an anode, and carrying out anode reaction under proper experimental conditions to obtain the titanium dioxide nano-ring. The obtained nano-ring has the advantages of favorable appearance, uniform size, low preparation cost and simple technological process, thus achieving industrialized mass production.
Description
Technical field
The invention belongs to nano material preparation technology and optoelectronic information field of materials, be specifically related to a kind of method for preparing nanometer titania ring through the anonizing big area fast.
Background technology
In recent years, emerging various nanometer annular materials are because of its unique physics, and chemical property is in transmitter, nanoelectronics and receive aspects such as Mechatronic Systems and have the potential application prospect and get more and more people's extensive concerning.Nanometer titania as a kind of material with property at photolysis water hydrogen, gas sensor, there is very big potentiality to be exploited aspects such as solar cell.
In the preparation method of existing nano-rings, the common more complicated of its preparation process also has a lot of technological difficulties to overcome simultaneously.The preparation method of the nanometer titania ring of announcing such as patent [200610130164.1] is with emulsion polymerisation process synthetic polystyrene nanometer ball, to pass through sol-gel process then at its surface coverage TiO
2Colloidal particle is removed the pipe/polyhenylethylene nano ball through thermal treatment again, obtains TiO
2Nano-rings.The limited size of its ring is in the pipe/polyhenylethylene nano ball, and the preparation process is more loaded down with trivial details, and technical difficulty is big.Also not useful anonizing prepares the correlative study report of nanometer titania ring at present.
Summary of the invention
The object of the present invention is to provide a kind of completely new approach that adopts anodic oxidation to prepare nanometer titania ring.This method adopts anonizing that the titanium sheet of chemical rightenning is handled, and through the regulation and control to conditions such as voltage, concentration and reaction times, forms the nano-rings structured material with advantageous property at last.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of anodic oxidation preparation method of nanometer titania ring specifically prepares process and carries out through the following step:
Step 1, raw materials pretreatment:
It is ultrasonic peace and quiet that the titanium sheet that cuts is put into acetone, then with putting into HF, HNO behind the deionized water rinsing
3And H
2Chemical rightenning is handled in the mixing solutions of O, and described mixed liquor volume is than being HF:HNO
3: H
2O=1:4:5, ultrasonic peace and quiet in ethanol then, then be kept in the ethanol for use;
Step 2, anodic oxidation reactions:
With the massfraction is the NH of 0.25wt%-0.50wt%
4The F ethanol solution is an electrolytic solution, and pretreated titanium sheet is an anode, and carbon-point is done negative electrode, and bath temperature is 20 ℃, and voltage is under the condition of 20v-60V, and anodic oxidation 2h-72h obtains nanometer titania ring.
Preferably, used ethanol is absolute ethyl alcohol in the step 1.
The present invention need not special instruments and equipment, and cost is low, and compared with prior art, the present invention has the following advantages:
(1) the present invention is based on anonizing and prepare nanometer titania ring, the preparation controllable process can be according to the adjustment voltage swing, reaction solution concentration, and the reaction times etc. are regulated and control the proterties of nano-rings.
(2) the nano-rings pattern of the present invention's preparation is good, and yardstick is even, and preparation cost is low, and flow process is succinct, can in industry, realize scale operation.
(3) the present invention can realize generating nanometer titania ring attached to the titanium film original position on the different base.
Description of drawings
Fig. 1 is ESEM (SEM) figure of gained sample among the embodiment 1;
Fig. 2 is the sem photograph of gained sample among the embodiment 2.
Below in conjunction with embodiment and accompanying drawing the present invention is done further detailed description.
Embodiment
The present invention prepares process and carries out with the following step:
Step 1, raw materials pretreatment
The titanium sheet that cuts is put into the acetone ultrasonic cleaning to remove raw material surface oil stain, then with putting into HF, HNO behind the deionized water rinsing
3And H
2Chemical rightenning is handled until the no longer alveolate violent generation of reaction in the mixing solutions of O, and described mixed liquor volume is than being HF:HNO
3: H
2O=1:4:5, ultrasonic cleaning then is kept in the ethanol for use to remove the solution of remained on surface in ethanol then; The all preferred absolute ethyl alcohol of used ethanol;
Step 2, anodic oxidation reactions
With the massfraction is the NH of 0.25wt%-0.50wt%
4The F ethanol solution is an electrolytic solution, and pretreated titanium sheet is an anode, and carbon-point is done negative electrode, and bath temperature is 20 ℃, and voltage is under the condition of 20v-60V, and anodic oxidation 2h-72h promptly obtains nanometer titania ring.
Below be the specific embodiment that the contriver provides, these embodiment are in order further to understand the present invention, to the invention is not restricted to these embodiment.
Embodiment 1:
Step 1, raw materials pretreatment:
Earlier the titanium sheet being cut out is 2cm * 4cm, in acetone, adds sonic oscillation and removes oil stain 5min, cleans up with deionized water, puts it into HF, HNO again
3And H
2Chemical rightenning is handled 10min and is no longer included bubble until reaction and acutely produce in the mixing solutions of O, and described mixed liquor volume is than being HF:HNO
3: H
2O=1:4:5, ultrasonic cleaning 3min in absolute ethyl alcohol then, it is residual to remove surface liquid, is kept in the absolute ethyl alcohol for use;
Step 2, anodic oxidation reactions
With the 100ml absolute ethyl alcohol is solvent, and the 0.1983g Neutral ammonium fluoride is a solute, and pretreated titanium sheet is an anode, and carbon-point is done negative electrode, and bath temperature is 20 ℃, and voltage is under the condition of 50v, and anodic oxidation 2h promptly obtains nanometer titania ring.
The SEM test result is as shown in Figure 1, and the size of ring is even, and the well-formed is shaped as oval nano-rings structure, and major axis is approximately 500nm, and minor axis is approximately 250nm.
Embodiment 2:
Step 1, raw materials pretreatment
Earlier the titanium sheet is cut out to 2cm * 4cm, in acetone, added sonic oscillation oil removing 5min, clean up, put it into HF, HNO again with deionized water
3And H
2Chemical rightenning is handled 10min until the no longer alveolate violent generation of reaction in the mixing solutions of O, and described mixed liquor volume is than being HF:HNO
3: H
2O=1:4:5, ultrasonic cleaning 3min in absolute ethyl alcohol then, it is residual to remove surface liquid, is kept in the absolute ethyl alcohol for use;
Step 2, anodic oxidation reactions
With the 100ml absolute ethyl alcohol is solvent, and the 0.1983g Neutral ammonium fluoride is a solute, and pretreated titanium sheet is an anode, and carbon-point is done negative electrode, and bath temperature is 20 ℃, and voltage is under the condition of 30v, and anodic oxidation 72h promptly obtains nanometer titania ring.
The SEM test result is as shown in Figure 2, and the size of ring is even, and the well-formed is shaped as circular nano-rings structure, and diameter is approximately 500nm, highly is approximately 500n.
Claims (1)
1. the anodic oxidation preparation method of a nanometer titania ring is characterized in that, said method is carried out through the following step:
Step 1, raw materials pretreatment:
Earlier the titanium sheet being cut out is 2cm * 4cm, in acetone, adds sonic oscillation and removes oil stain 5min, cleans up with deionized water, puts it into HF, HNO again
3And H
2Chemical rightenning is handled 10min and is no longer included bubble until reaction and acutely produce in the mixing solutions of O, and described mixed liquor volume is than being HF:HNO
3: H
2O=1:4:5, ultrasonic cleaning 3min in absolute ethyl alcohol then, it is residual to remove surface liquid, is kept in the absolute ethyl alcohol for use;
Step 2, anodic oxidation reactions
With the 100ml absolute ethyl alcohol is solvent, and the 0.1983g Neutral ammonium fluoride is a solute, and pretreated titanium sheet is an anode, and carbon-point is done negative electrode, and bath temperature is 20 ℃, and voltage is under the condition of 50v, and anodic oxidation 2h promptly obtains nanometer titania ring;
Perhaps,
Step 1, raw materials pretreatment
Earlier the titanium sheet is cut out to 2cm * 4cm, in acetone, added sonic oscillation oil removing 5min, clean up, put it into HF, HNO again with deionized water
3And H
2Chemical rightenning is handled 10min until the no longer alveolate violent generation of reaction in the mixing solutions of O, and described mixed liquor volume is than being HF:HNO
3: H
2O=1:4:5, ultrasonic cleaning 3min in absolute ethyl alcohol then, it is residual to remove surface liquid, is kept in the absolute ethyl alcohol for use;
Step 2, anodic oxidation reactions
With the 100ml absolute ethyl alcohol is solvent, and the 0.1983g Neutral ammonium fluoride is a solute, and pretreated titanium sheet is an anode, and carbon-point is done negative electrode, and bath temperature is 20 ℃, and voltage is under the condition of 30v, and anodic oxidation 72h promptly obtains nanometer titania ring.
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| CN2011100242755A CN102115903B (en) | 2011-01-22 | 2011-01-22 | Method for preparing titanium dioxide nano-ring through anodic oxidation |
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| CN102115903B true CN102115903B (en) | 2012-08-08 |
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| CN106283099B (en) * | 2016-08-25 | 2018-12-21 | 岭南师范学院 | A kind of method and its application of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and manganese dioxide nano-composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101785880A (en) * | 2009-12-31 | 2010-07-28 | 东南大学 | Blood vessel bracket utilizing titanium oxide nanotube to load medicine |
| CN101899701A (en) * | 2010-07-19 | 2010-12-01 | 西南交通大学 | Method for preparing composite material of copper sulfide and titanium dioxide nano-tube |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101785880A (en) * | 2009-12-31 | 2010-07-28 | 东南大学 | Blood vessel bracket utilizing titanium oxide nanotube to load medicine |
| CN101899701A (en) * | 2010-07-19 | 2010-12-01 | 西南交通大学 | Method for preparing composite material of copper sulfide and titanium dioxide nano-tube |
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