CN1528672A - Titanium oxide nano tube and preparing method thereof - Google Patents

Titanium oxide nano tube and preparing method thereof Download PDF

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CN1528672A
CN1528672A CNA031346863A CN03134686A CN1528672A CN 1528672 A CN1528672 A CN 1528672A CN A031346863 A CNA031346863 A CN A031346863A CN 03134686 A CN03134686 A CN 03134686A CN 1528672 A CN1528672 A CN 1528672A
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nanotube
titanium oxide
radical nanopipe
titanate radical
tio
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CN1258479C (en
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张中太
李俊荣
唐子龙
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Tsinghua University
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Tsinghua University
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Abstract

The invention relates to a Ti oxide nano tube and preparing method. Its character: using TiO2 of various crystal shapes as raw material, and making ultrasonic processing, hydrothermal reaction and after treatment in NaOH solution to obtain titanic acid nano tube, and then baking to form TiO2 nano tube with anatase structure. The TiO2 nano tube has uniform appearance, small tube diameter and large specific surface area. It has wide applied prospect in the fields of photocatalysis, environmental purification, solar cell, gas and wet sensitive materials, etc. It has low energy consumption, simple device, and easy controlled condition, easy to realize large-scale industrial production.

Description

A kind of titanium oxide nanotube and preparation method thereof
Technical field
The present invention relates to a kind of titanium oxide nanotube and preparation method thereof, belong to the nano material preparation technical field.
Background technology
1991, Japanese scientist Iijima found carbon nanotube, because carbon nanotube has special chemistry, physical and mechanical property, had caused various countries scientists' common concern.Carbon nanotube usually needs at high temperature to generate, behind carbon nanotube, the nano material with one-dimentional structure as: nanotube, nano wire, nanometer rod etc. have become the research focus.
TiO 2Be oxide semiconductor material, be with a wide range of applications TiO at aspects such as photochemical catalysis, environmental purification, support of the catalyst, lithium ion battery, gas sensor and solar cells with extensive use 2Three kinds of crystal formations are arranged, i.e. anatase octahedrite, rutile and brookite.Because TiO 2The popularity of using, people are exploring TiO always 2Synthesis technique to its pattern, structure and Effect on Performance.The preparation of titania nanotube is one of research focus of field of nano material preparation.
In recent years, several preparation TiO had been developed 2The method of nanotube is mainly template, organic gel method and electrochemistry anodic oxidation.
Template: C.R.Martin floods TiO with porous alumina formwork 2Colloidal sol has synthesized TiO 2Nanotube and nano wire (materials chemistry, Chemistry ofMaterials,, 9 volumes, 2544 pages in 1997).With the synthetic TiO of template 2The pattern of nanotube directly is subjected to the homogeneity of pore passage structure of template and the influence of thickness, synthesis technique is also very big to the influence of product simultaneously, condition control requires relatively harsher, for example, the form of product is very responsive to the time of dipping, obtain nanotube, and the time of dipping is very short, be generally several seconds, thereby be difficult to realize industrialized production.Dipping time is short more, and the tube wall that obtains is thin more, just can only obtain nano wire and prolong dipping time, and the nanotube that obtains is generally amorphous TiO 2, and its tube wall is made of nano particle usually, owing to be subjected to the restriction of template, the diameter of nanotube is bigger, and specific surface area is also smaller, and, it is raw material that sol-gel method needs expensive organic alkoxide usually, and the production cost height is not suitable for scale operation.
Organic gel method: organic alkoxide of human titaniums such as M.Adachi is a raw material, makes template with the organic ammonium tensio-active agent, has synthesized TiO through sol-gel process 2Nanotube (chemical news flash, Chemistry Letters,, 942 pages in 2000), this method technological process more complicated, condition control ratio are harsh, and the nanotube of preparation is generally amorphous structure, the raw materials used organism that mostly is, and relatively more expensive, be unsuitable for scale operation.
Electrochemistry anodic oxidation: recently, investigation of materials journal (Journal ofMaterials Research, calendar year 2001,16 volumes, 3331 pages) has reported that electricity consumption chemical anode oxidation style has prepared TiO 2Nano-tube array is used for air-sensitive or humidity-sensitive element, and the nanotube diameter of preparation is thicker, and tube wall is by nano-TiO 2Granulometric composition, specific surface area is smaller, has limited its Application Areas.
The cheap industrial various TiO of the present invention 2Powder be feedstock production diameter less and even, the TiO that specific surface area is bigger 2Nanotube, preparation is simple, raw material is cheap and easy to get, and the productive rate height is suitable for large-scale commercial production.
Summary of the invention
The object of the present invention is to provide a kind of diameter less, evenly, bigger length-to-diameter ratio is arranged, the preparation method of titanium oxide nanotube that specific surface area is big and the titanium oxide nanotube that the reaction conditions gentleness is controlled, energy consumption is low.
A kind of titanium oxide nanotube that the present invention proposes, it is characterized in that: this titanium oxide nanotube is the TiO with industrial various crystal formations 2Be raw material, in NaOH solution, through supersound process, hydro-thermal reaction and aftertreatment obtain titanate radical nanopipe, form through calcination process to have anatase structured titania nanotube again.
The preparation method of a kind of titanium oxide nanotube that the present invention proposes, it is characterized in that: this method is carried out successively as follows:
(1) earlier with TiO 2Press 1-5gTiO with the NaOH solution of 5～20 mol 2The mixed of per 40 milliliters of NaOH places ultrasonic generator, carries out the sonochemistry reaction;
(2) the reacted mixing solutions of sonochemistry is moved into carry out hydro-thermal reaction in the alkali proof encloses container then;
(3) white product that step (2) is obtained is neutralized to acidity with after excessive alkali separates with diluted acid, and ageing cleans up with deionized water, and with the dehydrated alcohol exchange, oven dry obtains titanate radical nanopipe, and its chemical formula is H 2Ti 3O 7H 2O;
(4) with the above-mentioned titanate radical nanopipe vacuum-drying that obtains, 250～400 ℃ of roastings can obtain TiO after 0.5～5 hour 2Nanotube.
In above-mentioned titanium oxide nanotube preparation method, the described ultrasonic power of step (1) is 0.2～100W/cm 2, temperature is 30～90 ℃, the time is 0.2～6 hour.
In above-mentioned titanium oxide nanotube preparation method, the described hydrothermal temperature of step (2) is 80～255 ℃, and the time is 4 hours to 96 hours.
The present invention adopts cheap industrial production TiO 2Be raw material, with sonochemical method and hydrothermal reaction at low temperature, the TiO of preparation 2Nanotube pattern homogeneous, caliber is little, and specific surface area is big.This product has in fields such as photochemical catalysis, environmental purification, solar cell, air-sensitive, humidity-sensitive materials extensively sends out application prospect.Sonochemical method is a kind of efficient height, energy consumption is low, speed is fast and eco-friendly chemical process, is called as " Green Chemistry process ", in conjunction with hydrothermal reaction at low temperature, the energy consumption of entire synthesis process is lower, equipment is simple, and condition is controlled easily, realizes large-scale commercial production easily.
Description of drawings
Fig. 1 is a raw material for the present invention adopts anatase crystal titanium dioxide, the transmission electron microscope figure of the titanate radical nanopipe of sonochemistry-Hydrothermal Preparation.
Fig. 2 is a raw material for the present invention adopts rutile crystal type titanium dioxide, the transmission electron microscope figure of the titanate radical nanopipe of sonochemistry-Hydrothermal Preparation.
Fig. 3 is the transmission electron microscope figure of titania nanotube of the present invention.
Fig. 4 is the high resolution transmission electron microscopy figure of titania nanotube of the present invention.
Fig. 5 is the X-ray powder diffraction figure of titanate radical nanopipe of the present invention.
Fig. 6 is the X-ray powder diffraction figure of titania nanotube of the present invention.
Fig. 7 is the X-ray powder diffraction figure of the present invention's two titanate radical nanopipes after 580 ℃ of roastings.
Embodiment
The present invention is a raw material with industrial various titanium dioxide at first, the preparation titanate radical nanopipe.In preparation process, make full use of cavitation effect of ultrasonic waves, material is pulverized, fully increase the contact area of titanium dioxide and alkali, simultaneously, the instantaneous local ultrahigh-temperature ultra-high voltage that utilizes ultrasonic wave to produce, the effect of having quickened titanium dioxide and alkali generates titanate.The titanate that generates has laminate structure, and flaky titanate crystal growth is rolled into the titanate nanotube with laminate structure then under hydrothermal condition.Titanate nanotube forms titanate radical nanopipe after strong acid exchange, neutralization.Titanate radical nanopipe has anatase structured titania nanotube through further handling to form.The inventive method preparation process technology is simple, the condition controllability is strong, and reaction is quick, energy consumption is low, and raw material is cheap and easy to get, productive rate is high, is easy to realize large-scale commercial production.
Preparation technology of the present invention mainly comprises following two aspects:
One, be the feedstock production titanate radical nanopipe with industrial titanium dioxide
This method for preparing titanate radical nanopipe makes full use of hyperacoustic porphyrization, and large granular materials fully is ground into fine particle, increases the contact area between the material, reduces the resistance to mass transfer of reaction; The instantaneous local ultrahigh-temperature ultra-high voltage that utilizes the ultrasonic cavitation effect to produce simultaneously, the carrying out of accelerated reaction utilizes low-temperature hydrothermal to carry out crystallization then, obtains titanate nanotube.Form titanate radical nanopipe through aftertreatment.
Processing step: the industrial titanium dioxide of 1～5 gram is mixed with the NaOH solution of 40 milliliter of 5～20 mol, place ultrasonic generator, carry out the sonochemistry reaction, 30～90 ℃ of temperature, ultrasonic power 0.2～100W/cm 2, 0.2～6 hour time; Move into then and carry out hydro-thermal reaction in the alkali proof encloses container, temperature is 80～255 ℃, time is 4 hours to 96 hours, and product with after excessive alkali separates, is neutralized to acidity with diluted acid, ageing 2～12 hours, use washed with de-ionized water, with the dehydrated alcohol exchange for several times, drying, obtain titanate radical nanopipe, its chemical formula is H 2Ti 3O 7H 2O.
Two, the titanate radical nanopipe with method for preparing is a raw material, and preparation has the titania nanotube of anatase crystal.
This synthetic TiO 2The method of nanotube utilizes the dry dehydration of metatitanic acid to generate the characteristics of titanium dioxide, after the drying process and roasting of certain temperature, certain vacuum degree, can be converted into the titania nanotube with anatase crystal by highly selective.
Processing step: at 60～120 ℃, vacuum-drying is 2～12 hours under the certain vacuum degree, 250～400 ℃ of following roastings 0.5～5 hour, can obtain titania nanotube then with the titanate radical nanopipe of above-mentioned preparation.
Below be embodiment with prepared titanate radical nanopipe of the present invention and titania nanotube.
Embodiment 1
The preparation of titanate radical nanopipe
Take by weighing the titania powder of the industrial anatase crystal of 1.0 grams, put into Erlenmeyer flask, add the NaOH solution of 40 milliliter of 10 mol, put into ultrasonic generator, ultrasonic temperature is 35 ℃, with 0.2W/cm 2Power ultrasonic 5 hours.Move into then in the autoclave of teflon lined of 50mL, 125 ℃ of hydro-thermal reactions 20 hours are with white product and excessive alkali centrifugation, with the HNO of 0.1 mol 3Being neutralized to the pH value is 2～6, and ageing is clean with rinsed with deionized water then, and with dehydrated alcohol exchange three times, drying can get titanate radical nanopipe again.Its molecular formula is H 2Ti 3O 7H2O.
Repeat the aforesaid operations step, ultrasonic temperature is 85 ℃, with 0.2W/cm 2Power ultrasonic can get titanate radical nanopipe in 2 hours.
Repeat the aforesaid operations step, ultrasonic temperature is 35 ℃, with 95W/cm 2Power ultrasonic can get titanate radical nanopipe in 0.5 hour.
Repeat the aforesaid operations step, ultrasonic temperature is 85 ℃, with 95W/cm 2Power ultrasonic can get titanate radical nanopipe in 0.2 hour.
Repeat the aforesaid operations step,, can get titanate radical nanopipe 245 ℃ of following hydro-thermal reactions 8 hours.
Repeat the aforesaid operations step,,, can get titanate radical nanopipe 245 ℃ of following hydro-thermal reactions 4 hours with the NaOH solution of 20 mol.
Repeat the aforesaid operations step,,, can get titanate radical nanopipe 80 ℃ of following hydro-thermal reactions 96 hours with the NaOH solution of 20 mol.
Repeat the aforesaid operations step,,, can get titanate radical nanopipe 245 ℃ of following hydro-thermal reactions 48 hours with the NaOH solution of 5 mol.
More than under arbitrary condition, add the 5g titania powder, can get titanate radical nanopipe.
Product detects through TEM and is nanotube (Fig. 1), about 8～10 nanometers of nanotube external diameter, and the about hundreds of nanometer of length is to micron order.Detecting product with the X-ray powder diffraction is titanate radical nanopipe.Use N 2Its BET specific surface area of determination of adsorption method is 394.9m 2/ g.
Embodiment 2
Take by weighing the titania powder of the industrial rutile crystal type of 1.0 grams, put into Erlenmeyer flask, add the NaOH solution of 40 milliliter of 10 mol, put into ultrasonic generator, with 0.2W/cm 2Power ultrasonic 5 hours, temperature is 85 ℃.Move into then in the autoclave of teflon lined of 50mL, 125 ℃ of hydro-thermal reactions 30 hours are with white product and excessive alkali centrifugation, with the HNO of 0.1 mol 3Being neutralized to the pH value is 2～6, and ageing 8 hours is clean with rinsed with deionized water then, and with dehydrated alcohol exchange three times, drying can get titanate radical nanopipe again.Its molecular formula is H 2Ti 3O 7H2O.
Repeat the aforesaid operations step, ultrasonic temperature is 85 ℃, with 0.2W/cm 2Power ultrasonic can get titanate radical nanopipe in 3 hours.
Repeat the aforesaid operations step, ultrasonic temperature is 35 ℃, with 95W/cm 2Power ultrasonic can get titanate radical nanopipe in 1 hour.
Repeat the aforesaid operations step, ultrasonic temperature is 85 ℃, with 95W/cm 2Power ultrasonic can get titanate radical nanopipe in 0.5 hour.
Repeat the aforesaid operations step,, can get titanate radical nanopipe 245 ℃ of following hydro-thermal reactions 12 hours.
Repeat the aforesaid operations step,,, can get titanate radical nanopipe 245 ℃ of following hydro-thermal reactions 6 hours with the NaOH solution of 20 mol.
Repeat the aforesaid operations step,,, can get titanate radical nanopipe 90 ℃ of following hydro-thermal reactions 96 hours with the NaOH solution of 20 mol.
Repeat the aforesaid operations step,,, can get titanate radical nanopipe 245 ℃ of following hydro-thermal reactions 72 hours with the NaOH solution of 5 mol.
More than under arbitrary condition, add the 5g titania powder, can get titanate radical nanopipe.
Product detects through TEM and is nanotube (Fig. 2), about 8～10 nanometers of nanotube external diameter, and the about hundreds of nanometer of length is to several microns.Detecting product with the X-ray powder diffraction is titanate radical nanopipe.
Embodiment 3
The preparation of titania nanotube
At 60 ℃, vacuum-drying is 12 hours under the vacuum tightness of 100Pa with the titanate radical nanopipe of above-mentioned preparation, then 250 ℃ of following roastings 5 hours, get final product titania nanotube.
Repeat above-mentioned steps, at 120 ℃, vacuum-drying is 8 hours under the vacuum tightness of 200Pa, can get titania nanotube.
Repeat above-mentioned steps, can get titania nanotube in 0.5 hour 400 ℃ of following roastings.
Product detects through TEM and is nanotube, and detecting product with the X-ray powder diffraction is the titanium dioxide of anatase crystal, uses N 2Its BET specific surface area of determination of adsorption method is 261.4m 2/ g.Fig. 3 is the transmission electron microscope figure of titania nanotube, and Fig. 4 is the high resolution transmission electron microscopy figure of titania nanotube, and Fig. 6 is the X-ray diffractogram of titania nanotube.
With the titanate radical nanopipe of above-mentioned preparation 580 ℃ of following roastings 2 hours, all change the titanic oxide nano powder of anatase crystal into, do not see that the crystalline phase that other titanate is arranged occurs, showing in the titanate radical nanopipe of preceding method preparation and the titania nanotube does not have residual alkalimetal ion.Fig. 7 is the X-ray diffractogram of anatase crystal titanic oxide nano.

Claims (4)

1, a kind of titanium oxide nanotube is characterized in that: this titanium oxide nanotube is the TiO with industrial various crystal formations 2Be raw material, in NaOH solution, through supersound process, hydro-thermal reaction and aftertreatment obtain titanate radical nanopipe, form through calcination process to have anatase structured titania nanotube again.
2, a kind of preparation method of titanium oxide nanotube as claimed in claim 1 is characterized in that: this method is carried out successively as follows:
(1) earlier with TiO 2Press 1-5gTiO with the NaOH solution of 5～20 mol 2The mixed of per 40 milliliters of NaOH places ultrasonic generator, carries out the sonochemistry reaction;
(2) the reacted mixing solutions of sonochemistry is moved into carry out hydro-thermal reaction in the alkali proof encloses container then;
(3) white product that step (2) is obtained is with after excessive alkali separates, and being neutralized to pH with diluted acid is 2-6, and ageing cleans up with deionized water, and with the dehydrated alcohol exchange, oven dry obtains titanate radical nanopipe, and its chemical formula is H 2Ti 3O 7H 2O;
(4) with the above-mentioned titanate radical nanopipe vacuum-drying that obtains, 250～400 ℃ of roastings can obtain TiO after 0.5～5 hour 2Nanotube.
3, according to the described method for preparing the titanium oxide nanotube of claim 1, it is characterized in that: the described ultrasonic power of step (1) is 0.2～100W/cm 2, temperature is 30～90 ℃, the time is 0.2～6 hour.
4, according to the described method for preparing the titanium oxide nanotube of claim 1, it is characterized in that: the described hydrothermal temperature of step (2) is 80～255 ℃, and the time is 4 hours to 96 hours.
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Cited By (26)

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CN1317193C (en) * 2005-07-07 2007-05-23 上海交通大学 Method for microwave preparation of titania nanometer tube
WO2008014690A1 (en) * 2006-07-27 2008-02-07 Beijing Xianxundongtai Technology Co., Ltd. A nano-wire of titania, a method for preparing the same, the use of the same, and a method for degradation of organic contaminants
CN100384742C (en) * 2004-12-15 2008-04-30 河南大学 Method for preparing nano-tubular sodium titanate/titanci acid
CN100465358C (en) * 2005-12-20 2009-03-04 中国科学院兰州化学物理研究所 Process of preparing oil soluble nano titania line
CN101504989A (en) * 2009-03-06 2009-08-12 清华大学 Titanium oxide energy accumulation cell with high power and high energy
CN101279762B (en) * 2008-05-26 2010-06-02 武汉理工大学 Preparation of fusiform anatase TiO2 nanocrystalline material
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CN101322943B (en) * 2007-06-15 2010-12-22 南京大学 Ti2O nano tube supported V2O5 composite catalyst
WO2011050516A1 (en) * 2009-10-27 2011-05-05 Chen Jun Method of testing titania nanotubes for adsorbing-degrading performances on micro-interface thereof
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CN102071461A (en) * 2010-11-19 2011-05-25 华南农业大学 Method for preparing titanium dioxide nanometer tubes and titanium dioxide nanometer tube preparation for loading enrofloxacin animal remedy
CN102350331A (en) * 2011-08-22 2012-02-15 浙江工业大学 Method for preparing TiO2 nanotube by ultrasound-hydrothermal reaction coupling
CN101633491B (en) * 2009-08-13 2012-06-20 重庆大学 Process for preparing titanium oxide nano tubes
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CN103395831A (en) * 2013-07-09 2013-11-20 哈尔滨工程大学 Hydrothermal preparation method of shape-controllable titanium dioxide nano tube
CN103553127A (en) * 2013-10-22 2014-02-05 渤海大学 Method for preparing anatase type titanium dioxide nano tube
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CN105347389A (en) * 2015-11-11 2016-02-24 湘潭大学 Ultra-thin titanate nanoribbons exposing (010) crystal face and preparation method thereof
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CN107973375A (en) * 2016-10-21 2018-05-01 苏州汉力新材料有限公司 One-dimensional Ag2The TiO of O nano wires modification2The preparation method of nanotube electrode
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CN100384742C (en) * 2004-12-15 2008-04-30 河南大学 Method for preparing nano-tubular sodium titanate/titanci acid
CN1317193C (en) * 2005-07-07 2007-05-23 上海交通大学 Method for microwave preparation of titania nanometer tube
CN100465358C (en) * 2005-12-20 2009-03-04 中国科学院兰州化学物理研究所 Process of preparing oil soluble nano titania line
WO2008014690A1 (en) * 2006-07-27 2008-02-07 Beijing Xianxundongtai Technology Co., Ltd. A nano-wire of titania, a method for preparing the same, the use of the same, and a method for degradation of organic contaminants
CN101319405B (en) * 2007-06-08 2011-05-18 中国科学院苏州纳米技术与纳米仿生研究所 Production method of TiO2 nanotube and/or TiO2 nano-whisker
CN101322943B (en) * 2007-06-15 2010-12-22 南京大学 Ti2O nano tube supported V2O5 composite catalyst
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CN101327949B (en) * 2008-05-26 2010-06-09 武汉理工大学 Preparation of one-dimensional titanate radical nanopipe material and use thereof
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CN101633491B (en) * 2009-08-13 2012-06-20 重庆大学 Process for preparing titanium oxide nano tubes
WO2011050516A1 (en) * 2009-10-27 2011-05-05 Chen Jun Method of testing titania nanotubes for adsorbing-degrading performances on micro-interface thereof
CN102071461A (en) * 2010-11-19 2011-05-25 华南农业大学 Method for preparing titanium dioxide nanometer tubes and titanium dioxide nanometer tube preparation for loading enrofloxacin animal remedy
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CN102350331A (en) * 2011-08-22 2012-02-15 浙江工业大学 Method for preparing TiO2 nanotube by ultrasound-hydrothermal reaction coupling
CN103288126A (en) * 2013-05-14 2013-09-11 哈尔滨工程大学 Method of preparing titanium dioxide nanotube with assistance of cationic surface active agent
CN103395831A (en) * 2013-07-09 2013-11-20 哈尔滨工程大学 Hydrothermal preparation method of shape-controllable titanium dioxide nano tube
CN103553127A (en) * 2013-10-22 2014-02-05 渤海大学 Method for preparing anatase type titanium dioxide nano tube
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