CN101037229A - Preparation method of TiO2 nano material using anode alumina as template by sol-gel process - Google Patents
Preparation method of TiO2 nano material using anode alumina as template by sol-gel process Download PDFInfo
- Publication number
- CN101037229A CN101037229A CNA2007100988618A CN200710098861A CN101037229A CN 101037229 A CN101037229 A CN 101037229A CN A2007100988618 A CNA2007100988618 A CN A2007100988618A CN 200710098861 A CN200710098861 A CN 200710098861A CN 101037229 A CN101037229 A CN 101037229A
- Authority
- CN
- China
- Prior art keywords
- template
- tio
- mixed solution
- active agent
- tio2
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to the metal material field, and relates to a preparation method of TiO2 nanometer material by sol gel method using anode aluminum oxide as a template. The present invention is characterized in that: the cetyl trimethyl ammonium bromide serves as the surface active agent, soft templates of different shapes are formed by changing the dosage of the surface active agent, combining with the characteristics of the even aperture of the hard template, the nanometer TiO2 tubular/linear material with fixed aperture is obtained. The appearance of the TiO2 nanometer material is attributed by TEM, which certifies that the production of nanometer TiO2 tubular/linear material can be controlled only by changing the dosage of the surface active agent CTAB; the obtained material is certified to be TiO2 material with polycrystalline state by XRD method. The method of the present invention is simple and is easy to be carried out.
Description
Technical field:
The invention belongs to metal material field, particularly a kind of is that template is utilized Prepared by Sol Gel Method TiO with the anodised aluminium
2The method of nano material.
Background technology:
Therefore AAO (anodised aluminium, Anodic Aluminum Oxide) template is widely used in the nano materials research because preparation technology is simple, and pore size is evenly adjustable.Under different purposes and environment for use, also different for the size of nano material with the pattern requirement, with TiO
2Be example: in antibiotic, need TiO
2Mostly be solid attitude, and in photocatalysis to degrade organic matter, improve TiO because need to add sensitizing agent
2Catalytic performance, so need TiO usually
2Be tubulose.Past is for the research of resultant pattern regulation and control, more mostly is to utilize complicated method regulation and control resultant pattern or only pay close attention to the regulation and control of resultant pattern and the size of resultant is not set forth.Under same preparation method, be that template is that adjustable product is that different-shape and the nano material with constant aperture size are not appeared in the newspapers by simple change preparation condition with AAO.
According to Lanzhou University's journal, 2003,39 (5): the 57-60 report: people such as Xu Hui find can prepare by factors such as the temperature of the immersion time of control AAO template and colloidal sol, concentration the nanotube and the line of different apertures and length.Need the multiple factor of control complicated in the preparation of reality, practical value is little.
Summary of the invention
The objective of the invention is to form difform soft template and in conjunction with the characteristics of AAO hard template uniform pore size, the nano-TiO with constant aperture size is prepared in regulation and control by the add-on that changes tensio-active agent
2Tubulose or filamentary material.
A kind of is that template is utilized Prepared by Sol Gel Method TiO with the anodised aluminium
2The method of material is characterized in that preparing the nano-TiO with constant aperture size by the add-on of regulation and control tensio-active agent cetyl trimethylammonium bromides (CTAB)
2Tubulose or filamentary material, concrete steps are:
Tetrabutyl titanate and dehydrated alcohol are made into 1. number mixed solution with 1: 5 mixed, and then get dehydrated alcohol, deionized water, hydrochloric acid and be made into 2. number mixed solution with 25: 1: 0.2 mixed.In ice-water bath, magnetic agitation is 1. behind number mixed solution 8-15min, will be 2. number mixed solution slowly join 1. in number mixed solution, and to add with respect to 1.+2. mixed solution massfraction be the tensio-active agent cetyl trimethylammonium bromide (CTAB) of 0.02%-0.39%, after keeping the constant continuation of rotating speed to stir 9-15min, stop to stir, promptly make TiO
2Vitreosol.The AAO template is immersed TiO
2Take out template behind the vitreosol 15-30min, at room temperature template left standstill 120-180min, be put in then in the retort furnace be warming up to 500-700 ℃ and constant temperature 240-300min with stove after, reduce to room temperature with stove.With massfraction is that 5% NaOH solution dissolves the AAO template, and that prepare generation is TiO
2Nanotube.
Prepare TiO according to above-mentioned steps
2The method of nano material, the add-on that it is characterized in that tensio-active agent cetyl trimethylammonium bromide (CTAB) are 1.+2. 0.4-4% of mixed solution massfraction, and that prepare generation is TiO
2Nano wire.
The research of sol-gel method Regulation Mechanism
By change method that the tensio-active agent add-on regulates and control prepared appearance of nano material mainly due to: the hydrolysis reaction equation of tetrabutyl titanate is: Ti (OC
4H
9)
4+ 6H
2O → Ti (OH)
6 2-+ 4C
4H
9OH+2H
+OH
-Mainly be adsorbed in TiO
2The gel particle surface makes it electronegative because the Surfactant CTAB that added is the cats product of positively charged, it can with Ti (OH)
6 2-Because electrostatic interaction forms compound body CTA
+-Ti (OH)
6 2-The geometry arrangement of CTAB molecule causes forming difform micelle, because surfactant molecule generally all is to be made of hydrophilic group and hydrophobic group, hydrophilic group when forming aggregate in the aggregate and hydrophobic group abut against together respectively and align.So that amphiphile, amphiphilic molecule aligns when forming aggregate, obtain difform aggregate along with the different of hydrophilic segment and hydrophobic part area occupied relative size.When the CTAB add-on more after a little while, the hydrophilic group CTA of positively charged
+Arrange easilier in the excellent type micellar of form outer.Because electrostatic interaction Ti (OH)
6 2-Along CTA
+The extension aligned growth, become TiO
2Nanotube.Otherwise, when the CTAB add-on is big, the hydrophilic group CTA of positively charged
+The easier arrangement on the interior edge of pointing to the center of circle forms anti-excellent type micelle.Ti (OH)
6 2-Along CTA
+Interior along aligned growth, become TiO
2Nano wire.
Characteristics of the present invention are to form difform soft template and in conjunction with the characteristics of AAO hard template uniform pore size, the nano-TiO with constant aperture size is prepared in regulation and control by the add-on that changes tensio-active agent
2Tubulose or filamentary material.Characterize TiO with TEM
2The pattern of nano material has confirmed to be adjustable generation nano-TiO by the add-on that changes Surfactant CTAB only
2Tubulose or filamentary material utilize the XRD means to confirm the nano material the generated TiO for polycrystalline state
2Material.This method is simple and practical, implements easily.
Description of drawings
Fig. 1 is the TiO of example 1 preparation
2Nanotube TEM figure.
Fig. 2 is the TiO of example 3 preparations
2Nano wire TEM figure.
Fig. 3 is corresponding to TiO
2The XRD figure of nano material/AAO composite structure
Embodiment
Example 1 Prepared by Sol Gel Method TiO
2Nanotube:
The 5mL tetrabutyl titanate is mixed (1. number mixed solution) with the 25mL dehydrated alcohol, and then get tensio-active agent cetyl trimethylammonium bromide (CTAB) mixing (2. number mixed solution) of 25mL dehydrated alcohol, 1mL deionized water, 0.2mL hydrochloric acid and 0.1g.In ice-water bath, magnetic agitation is 1. behind the 10min, will 2. slowly join 1., keep the constant continuation of rotating speed to stir 10min after, stop to stir, promptly make TiO
2Vitreosol.Take out template after the AAO template immersed this colloidal sol 15min, at room temperature template left standstill 120min, be put in then in the retort furnace be warming up to 700 ℃ and constant temperature 240min with stove after, reduce to room temperature with stove.With massfraction is that 5% NaOH solution dissolves the AAO template, prepares the TiO of generation
2Nanotube.
Example 2 Prepared by Sol Gel Method TiO
2Nanotube:
The 5mL tetrabutyl titanate is mixed (1. number mixed solution) with the 25mL dehydrated alcohol, and then get tensio-active agent cetyl trimethylammonium bromide (CTAB) mixing (2. number mixed solution) of 25mL dehydrated alcohol, 1mL deionized water, 0.2mL hydrochloric acid and 0.05g.In ice-water bath, magnetic agitation is 1. behind the 9min, will 2. slowly join 1., keep the constant continuation of rotating speed to stir 10min after, stop to stir, promptly make TiO
2Vitreosol.Take out template after the AAO template immersed this colloidal sol 18min, at room temperature template left standstill 150min, be put in then in the retort furnace be warming up to 700 ℃ and constant temperature 300min with stove after, reduce to room temperature with stove.With massfraction is that 5% NaOH solution dissolves the AAO template, prepares the TiO of generation
2Nanotube.
Example 3 Prepared by Sol Gel Method TiO
2Nano wire:
The 5mL tetrabutyl titanate is mixed (1. number mixed solution) with the 25mL dehydrated alcohol, and then get the CTAB mixing (2. number mixed solution) of 25mL dehydrated alcohol, 1mL deionized water, 0.2mL hydrochloric acid and 1.0g.In ice-water bath, magnetic agitation is 1. behind the 10min, will 2. slowly join 1., keep the constant continuation of rotating speed to stir 10min after, stop to stir, promptly make TiO
2Vitreosol.Take out template after the AAO template immersed this colloidal sol 15min, at room temperature template left standstill 120min, be put in then in the retort furnace be warming up to 700 ℃ and constant temperature 240min with stove after, reduce to room temperature with stove.With massfraction is that 5% NaOH solution dissolves the AAO template, prepares the TiO of generation
2Nano wire.
Example 4 Prepared by Sol Gel Method TiO
2Nano wire:
The 5mL tetrabutyl titanate is mixed (1. number mixed solution) with the 25mL dehydrated alcohol, and then get the CTAB mixing (2. number mixed solution) of 25mL dehydrated alcohol, 1mL deionized water, 0.2mL hydrochloric acid and 1.6g.In ice-water bath, magnetic agitation is 1. behind the 8min, will 2. slowly join 1., keep the constant continuation of rotating speed to stir 12min after, stop to stir, promptly make TiO
2Vitreosol.Take out template after the AAO template immersed this colloidal sol 15min, at room temperature template left standstill 150min, be put in then in the retort furnace be warming up to 600 ℃ and constant temperature 280min with stove after, reduce to room temperature with stove.With massfraction is that 5% NaOH solution dissolves the AAO template, prepares the TiO of generation
2Nano wire.As can be seen from the figure Fig. 1 is translucent nanotube, and Fig. 2 is the nano wire of opaque shape.TiO
2Nanotube and nanowire diameter all are about 100nm, and be consistent with its pore size of template, and whole smooth homogeneous.These nanotubes, line are made up of tiny nano particle.
From Fig. 3 corresponding to TiO
2The XRD figure of nano material/AAO composite structure is TiO as can be seen
2And Al
2O
3Characteristic peak, illustrate in the AAO template, successfully to make nano-TiO
2Material, and obtained nano-TiO
2Material is a polycrystalline state.
Claims (2)
1, a kind of is that template is utilized Prepared by Sol Gel Method TiO with the anodised aluminium
2The method of material is characterized in that tetrabutyl titanate and dehydrated alcohol are made into 1. number mixed solution with 1: 5 mixed, and then gets dehydrated alcohol, deionized water, hydrochloric acid and be made into 2. number mixed solution with 25: 1: 0.2 mixed; In ice-water bath, magnetic agitation is 1. behind number mixed solution 8-15min, will be 2. number mixed solution join 1. in number mixed solution, and to add with respect to 1.+2. mixed solution massfraction be the tensio-active agent cetyl trimethylammonium bromide of 0.02%-0.39%, after keeping the constant continuation of rotating speed to stir 9-15min, stop to stir, promptly make TiO
2Vitreosol; The AAO template is immersed TiO
2Take out template behind the vitreosol 15-30min, at room temperature template left standstill 120-180min, be put in then in the retort furnace be warming up to 500-700 ℃ and constant temperature 240-300min with stove after, reduce to room temperature with stove; With massfraction is that 5% NaOH solution dissolves the AAO template, and that prepare generation is TiO
2Nanotube.
2, a kind of according to claim 1 is that template is utilized Prepared by Sol Gel Method TiO with the anodised aluminium
2The method of material, the add-on that it is characterized in that the tensio-active agent cetyl trimethylammonium bromide are 1.+2. 0.4-4% of mixed solution massfraction, and that prepare generation is TiO
2Nano wire.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100988618A CN101037229A (en) | 2007-04-28 | 2007-04-28 | Preparation method of TiO2 nano material using anode alumina as template by sol-gel process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100988618A CN101037229A (en) | 2007-04-28 | 2007-04-28 | Preparation method of TiO2 nano material using anode alumina as template by sol-gel process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101037229A true CN101037229A (en) | 2007-09-19 |
Family
ID=38888437
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007100988618A Pending CN101037229A (en) | 2007-04-28 | 2007-04-28 | Preparation method of TiO2 nano material using anode alumina as template by sol-gel process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101037229A (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093048A (en) * | 2010-10-28 | 2011-06-15 | 广东工业大学 | Method for preparing perovskite ferroelectric nano tube array |
| CN102433978A (en) * | 2011-09-07 | 2012-05-02 | 南昌大学 | Novel nanometer titanium dioxide self-cleaning fluorine-carbon aluminum single sheet as well as low-temperature preparation method and application thereof |
| CN102502484A (en) * | 2011-09-28 | 2012-06-20 | 重庆大学 | Modified titanium dioxide nano particle nanotube and preparation method thereof |
| CN103614760A (en) * | 2013-11-27 | 2014-03-05 | 天津大学 | Method for preparing titanium dioxide nanotubes by utilizing secondary anodized aluminum oxide template |
| CN105036188A (en) * | 2015-07-07 | 2015-11-11 | 上海理工大学 | Titanium dioxide nanowire and preparation method thereof |
| CN106390975A (en) * | 2016-09-26 | 2017-02-15 | 常州大学 | Method for preparing barium titanate nanotube array |
| CN107200350A (en) * | 2017-07-11 | 2017-09-26 | 河南师范大学 | TiO is prepared by template of corn stigma2The method of nano-tube array catalysis material |
| CN107217286A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| CN107217288A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| CN107217285A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| CN107217276A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| CN109293944A (en) * | 2018-10-26 | 2019-02-01 | 浙江海洋大学 | A kind of preparation method of high-molecular polyivnyl alcohol nanometer grass |
| CN110877916A (en) * | 2019-11-27 | 2020-03-13 | 新疆众和股份有限公司 | Method for producing tubular titanium dioxide |
-
2007
- 2007-04-28 CN CNA2007100988618A patent/CN101037229A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093048A (en) * | 2010-10-28 | 2011-06-15 | 广东工业大学 | Method for preparing perovskite ferroelectric nano tube array |
| CN102433978A (en) * | 2011-09-07 | 2012-05-02 | 南昌大学 | Novel nanometer titanium dioxide self-cleaning fluorine-carbon aluminum single sheet as well as low-temperature preparation method and application thereof |
| CN102433978B (en) * | 2011-09-07 | 2015-05-20 | 南昌大学 | Novel nanometer titanium dioxide self-cleaning fluorine-carbon aluminum single sheet as well as low-temperature preparation method and application thereof |
| CN102502484A (en) * | 2011-09-28 | 2012-06-20 | 重庆大学 | Modified titanium dioxide nano particle nanotube and preparation method thereof |
| CN102502484B (en) * | 2011-09-28 | 2014-05-28 | 重庆大学 | Modified titanium dioxide nano particle nanotube and preparation method thereof |
| CN103614760A (en) * | 2013-11-27 | 2014-03-05 | 天津大学 | Method for preparing titanium dioxide nanotubes by utilizing secondary anodized aluminum oxide template |
| CN105036188B (en) * | 2015-07-07 | 2017-03-01 | 上海理工大学 | A kind of titanium dioxide nano thread and preparation method thereof |
| CN105036188A (en) * | 2015-07-07 | 2015-11-11 | 上海理工大学 | Titanium dioxide nanowire and preparation method thereof |
| CN106390975A (en) * | 2016-09-26 | 2017-02-15 | 常州大学 | Method for preparing barium titanate nanotube array |
| CN106390975B (en) * | 2016-09-26 | 2018-12-04 | 常州大学 | A kind of preparation method of Characterization of Barium Titanate Nanotubes array |
| CN107217286A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| CN107217288A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| CN107217285A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| CN107217276A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| CN107200350A (en) * | 2017-07-11 | 2017-09-26 | 河南师范大学 | TiO is prepared by template of corn stigma2The method of nano-tube array catalysis material |
| CN109293944A (en) * | 2018-10-26 | 2019-02-01 | 浙江海洋大学 | A kind of preparation method of high-molecular polyivnyl alcohol nanometer grass |
| CN110877916A (en) * | 2019-11-27 | 2020-03-13 | 新疆众和股份有限公司 | Method for producing tubular titanium dioxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101037229A (en) | Preparation method of TiO2 nano material using anode alumina as template by sol-gel process | |
| CN100998937B (en) | Fluorine doped-anatase type TiO2 collosol photo catalyst preparation method | |
| CN102500351B (en) | Nano composite laminated film based on TiO2 and preparation method thereof | |
| CN101792117B (en) | Method for preparing tungsten-doped anatase type nano titanium dioxide composite powder | |
| CN1583332A (en) | Nanometer silver sol and preparing method thereof | |
| CN108295830B (en) | TiO with 001, 101 crystal face exposed2Sepiolite composite gel and preparation method thereof | |
| CN1903948A (en) | In situ cladding technology of titanium dioxide nano-particle | |
| CN102583255B (en) | Method for preparing mesoporous composite transition metal oxide | |
| CN108817414B (en) | Preparation method of gold nanoflower in ionic liquid aqueous solution | |
| CN100480439C (en) | Method for preparing TiO2 nano material by direct current deposition method using anode aluminum oxide as template | |
| CN101074112A (en) | Production of high-purity superfine titanic oxide | |
| CN1803352A (en) | Method for preparing nanometer copper | |
| CN104192899A (en) | Method for preparing TiO2 nanocrystal particles | |
| CN103691433A (en) | Ag-doped TiO2 material, and preparation method and application thereof | |
| CN102358964A (en) | Method for preparing titanium-tungsten compound oxide nano-fiber | |
| CN104609465B (en) | The method that a kind of Barium metatitanate. doping multi-walled carbon nano-tubes prepares hud typed high dielectric filler | |
| CN103626227A (en) | Rutile type titanium dioxide micro-nano material and preparation method and application thereof | |
| Chen et al. | Recent advances in brookite phase TiO2-based photocatalysts toward CO2 reduction | |
| CN112058260B (en) | Preparation of core-shell structure Ag/TiO at normal temperature 2 Method for preparing nanoparticles and application thereof | |
| Darbandi et al. | Nanoscale engineering of TiO2 nanoparticles: Evolution of the shape, phase, morphology, and facet orientation | |
| CN107814412A (en) | A kind of particle morphology is the synthetic method of bar-shaped rutile type nano titanic oxide | |
| Karthikeyan et al. | Chemical methods for synthesis of hybrid nanoparticles | |
| Dalvandi et al. | Synthesis of titanium dioxide nano-powder via sol–gel method at ambient temperature | |
| CN111589460A (en) | W18O49BiOX composite photocatalytic material and preparation method thereof | |
| CN101117525A (en) | Intelligent film coating material and method for making same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |