CN102191529A - Honeycomb ordered titanium dioxide nanotube array film and preparation method thereof - Google Patents
Honeycomb ordered titanium dioxide nanotube array film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a honeycomb ordered titanium dioxide nanotube array film and a preparation method thereof. The honeycomb ordered titanium dioxide nanotube array film consists of an upper-layer ordered structure and a lower-layer ordered structure, namely an upper-layer large-diameter regular hexagonal titanium dioxide nanopore array and a lower-layer small-diameter titanium dioxide nanotube array, wherein a low-layer nanotube orifice end is positioned in upper-layer titanium dioxide nanopores and the upper-layer nanopores are communicated so as to form a honeycomb structure. The method is easy to operate, equipment is cheap, and parameters of the structure can be effectively controlled by changing the oxidation voltage and the oxidation time of an anode; moreover, titanium dioxide with the hierarchical structure can be widely applied to dye-sensitized solar cells, gas sensors, hydrogen preparation from water by photodecomposition, and photonic crystals.
Description
Technical field
The present invention relates to a kind of pervasive electrochemistry anodic oxidation, be used to prepare a kind of novel fractionated nanometer titania nano-tube array, be specifically related to a kind of cellular orderly film of Nano tube array of titanium dioxide and preparation method thereof.
Background technology
Pure titanium sheet (is mainly the organic or inorganic ionogen of fluoride ion) in some dielectric medium, can obtain the Nano tube array of titanium dioxide of ordered arrangement by anodic oxidation.These are by the Nano tube array of titanium dioxide of anonizing preparation, because of its unique tubular structure, high specific surface area and orderly arrangement mode, it are being had broad application prospects at environment, the energy, biology and optical field.In recent years, people mainly comprise the relation between oxidation voltage, oxidization time and electrolyte ingredient and concentration and titanium dioxide caliber, the pipe range always in the relation of seeking untiringly between electrochemical anodic oxidation parameter and the Nano tube array of titanium dioxide pattern.Yet used these work all concentrate on straight Nano tube array of titanium dioxide, i.e. the titania nanotube that all equates to the diameter of managing the bottom from the pipe top.Along with the development of nano science, this Nano tube array of titanium dioxide that only has single diameter perhaps can not satisfy the application demand of reality fully.Therefore probe into a kind of easy, effective synthetic method, the preparation complex structure, the Novel Titanium dioxide nanotube of controllable parameters is with significant.
Summary of the invention
It is cheap that the present invention is intended to develop a kind of equipment, and the simple efficient synthesis of working method is used to prepare the controlled novel nano structure titanium dioxide of structural parameter and constructs.
The present invention adopts following technical scheme to achieve these goals:
Cellular orderly film of Nano tube array of titanium dioxide is characterized in that:
Described cellular orderly film of Nano tube array of titanium dioxide is made up of upper and lower two-layer titanium dioxide nano-pore, and is supported on the titanium sheet substrate;
Described upper strata titanium dioxide nano-pore is orderly regular hexagon array, and its aperture is 70-250nm;
Described lower floor titanium dioxide nano-pore is real to be titania nanotube, and its opening end is to be arranged in the upper strata nanoporous, and each tube opening end is bonded to each other in the axial direction, and the aperture in lower floor hole is 15-40nm, and the degree of depth is 100-2000nm.
The preparation method of described cellular orderly film of Nano tube array of titanium dioxide is characterized in that may further comprise the steps:
(1) at first pure titanium sheet is put into that ultrasonic cleaning 55-65min removes the organism on surface in the mixing solutions of ethanol and acetone, and then cleaned repeatedly, and dry with deionized water;
(2) the titanium sheet after cleaning is dried is put into the ethylene glycol solution that contains 0.2mol/l hydrofluoric acid and is carried out anodic oxidation, and wherein oxidation voltage is 40-105v, and oxidization time is 1.2-1.5h, and titanium plate surface forms Nano tube array of titanium dioxide;
(3) will in hydrofluoric acid ethylene glycol ionogen, take out by anodised titanium sheet, place dehydrated alcohol, and, make the Nano tube array of titanium dioxide of titanium plate surface be removed by sonic oscillation, on titanium sheet substrate, stay the circular titanium dioxide nano-pore of ordered arrangement;
(4) preparation contains the ethylene glycol ionogen of 0.26mol/l Neutral ammonium fluoride, and will put into this ionogen through the titanium sheet after step (3) processing and carry out the anodic oxidation second time, its oxidation voltage is 15-30v, oxidization time is 10-70min, generate the more Nano tube array of titanium dioxide of minor diameter in the circular titanium dioxide nano-pore that this anode oxidation process can obtain in step (3), the circular titanium dioxide nano-pore enlarged-diameter of the middle acquisition of step (3) simultaneously, and circular port is transformed into the regular hexagon hole, thereby forms cellular orderly film of Nano tube array of titanium dioxide on the titanium sheet.
The preparation method of described cellular orderly film of Nano tube array of titanium dioxide is characterized in that: obtain by titanium sheet two-step electrochemical anodic oxidation treatment in the ethylene glycol organic electrolyte solution of hydrofluoric acid containing, Neutral ammonium fluoride.
The preparation method of described cellular orderly Nano tube array of titanium dioxide, it is characterized in that: by changing an anodic oxidation voltage from 40-105v, can make the Nano tube array of titanium dioxide of 50-120nm diameter range, after the ultrasonic vibration processing, can obtain the circular titanium dioxide nano-pore array of diameter range at 60-180nm.
The preparation method of described cellular orderly film of Nano tube array of titanium dioxide, it is characterized in that: during two-step anodization voltage, by changing oxidation voltage from 15-30v, can in the nanohole array after once oxidation is handled, make the Nano tube array of titanium dioxide of 15-40nm diameter range, obtain circular nanoporous enlarged-diameter after the anodic oxidation simultaneously to 70-250nm, and circular port is transformed into the regular hexagon hole, thereby forms cellular orderly film of Nano tube array of titanium dioxide.
The preparation method of described cellular orderly film of Nano tube array of titanium dioxide, it is characterized in that: when two-step anodization voltage, by changing oxidization time, can control secondary oxidation and make titania nanotube length between 100-2000nm from 10-70min.
In fact, the present invention adopts simple electrochemical apparatus, in conjunction with cheap electrochemical anodic oxidation technology, the cellular titania nanotube oldered array film that has synthesized the structure controllable parameters at ambient temperature, this structure is assembled by the titania nanotube of different tube diameters, prepare cellular orderly titanium dioxide nano material with this method, can reach the parameter that oxidization time just can be controlled this structure effectively by changing anodic oxidation voltage.
Beneficial effect of the present invention:
The present invention adopts simple electrochemical apparatus, in conjunction with cheap electrochemical anodic oxidation technology, has synthesized the nano-porous films that is made of cellular ordered arrangement titania nanotube at ambient temperature, and this novel nano structure has controllable size; Institute's employing method is simple to operate, equipment is cheap, can pass through to change electrolyte ingredient or concentration, and by changing anodic oxidation voltage, oxidization time, just can control the parameter of this structure effectively; This hierarchy titanium dioxide can be widely used aspect dye sensitization solar battery, gas sensor, photolysis water hydrogen and the photonic crystal.
Description of drawings
Fig. 1 prepares the process synoptic diagram of cellular orderly film of Nano tube array of titanium dioxide for the present invention.
Wherein figure (a) is the Nano tube array of titanium dioxide of anodic oxidation preparation, figure (b) stays the titanium dioxide nano-pore array on the titanium sheet substrate after for the titania nanotube that removes anodic oxidation preparation, and figure (c) be the cellular orderly film of Nano tube array of titanium dioxide for preparing by two-step anodization.
Fig. 2 prepares the microtexture and the characterization result of cellular each process correspondence of orderly film of Nano tube array of titanium dioxide by anodic oxidation for the present invention.
Figure (a) is the Nano tube array of titanium dioxide of anodic oxidation preparation, figure (b) is the titanium dioxide nano-pore oldered array that stays after the Nano tube array of titanium dioxide that an anodic oxidation generates is removed, figure (c) is the cellular orderly film of Nano tube array of titanium dioxide top SEM figure by the two-step anodization preparation, and figure (d) is the side SEM figure of cellular orderly film of Nano tube array of titanium dioxide.
Fig. 3 is in the hydrofluoric acid ethylene glycol ionogen of 0.2M, behind the titanium dioxide nano-pore array that the 100v oxidation voltage obtains down, and the cellular orderly film of Nano tube array of titanium dioxide that after carrying out secondary oxidation under the different voltages, prepares.
The sample that figure (a) prepares down for the 15v oxidation voltage, wherein hole diameter is 17nm; The sample that figure (b) prepares down for the 20v oxidation voltage, wherein hole diameter is 24nm; The sample that figure (c) prepares down for the 25v oxidation voltage, wherein hole diameter is 31nm; The sample that figure (d) prepares down for the 30v oxidation voltage, wherein hole diameter be 39nm. wherein the upper right corner of each figure be the partial enlarged drawing sheet.
Embodiment
The cellular orderly film of Nano tube array of titanium dioxide of embodiment, described cellular orderly titania nanotube shape array film is made up of upper and lower two-layer titanium dioxide nano-pore, and is supported on the titanium sheet substrate;
Described upper strata titanium dioxide nano-pore is orderly regular hexagon array, and its aperture is 70-250nm;
Described lower floor titanium dioxide nano-pore is real to be titania nanotube, and its opening end is to be arranged in the upper strata nanoporous, and each tube opening end is bonded to each other in the axial direction, and the aperture in lower floor hole is 15-40nm, and the degree of depth is 100-2000nm.
The preparation method of cellular orderly film of Nano tube array of titanium dioxide may further comprise the steps:
(1) at first pure titanium sheet is put into that ultrasonic cleaning 55-65min removes the organism on surface in the mixing solutions of ethanol and acetone, and then cleaned repeatedly, and dry with deionized water;
(2) the titanium sheet after cleaning is dried is put into the ethylene glycol solution that contains 0.2mol/l hydrofluoric acid and is carried out anodic oxidation, and wherein oxidation voltage is 40-105v, and oxidization time is 1.2-1.5h, and titanium plate surface forms Nano tube array of titanium dioxide;
(3) will in hydrofluoric acid ethylene glycol ionogen, take out by anodised titanium sheet, place dehydrated alcohol, and, make the Nano tube array of titanium dioxide of titanium plate surface be removed by sonic oscillation, on titanium sheet substrate, stay the circular titanium dioxide nano-pore of ordered arrangement;
(4) preparation contains the ethylene glycol ionogen of 0.26mol/l Neutral ammonium fluoride, and will put into this ionogen through the titanium sheet after step (3) processing and carry out the anodic oxidation second time, its oxidation voltage is 15-30v, oxidization time is 10-70min, generate the more Nano tube array of titanium dioxide of minor diameter in the circular titanium dioxide nano-pore that this anode oxidation process can obtain in step (3), the circular titanium dioxide nano-pore enlarged-diameter of the middle acquisition of step (3) simultaneously, and circular port is transformed into the regular hexagon hole, thereby forms cellular orderly film of Nano tube array of titanium dioxide on the titanium sheet.
Obtain by the twice electrochemical anodic oxidation processing in the ethylene glycol organic electrolyte solution of hydrofluoric acid containing, Neutral ammonium fluoride of titanium sheet.
By changing an anodic oxidation voltage from 40v-105v, can make the Nano tube array of titanium dioxide of 50-120nm scope diameter, after handling by ultrasonic vibration, can obtain the titanium dioxide nano-pore array of diameter range at 60-180nm.
During two-step anodization voltage, by changing oxidation voltage from 15v-30v, can in the nanohole array after once oxidation is handled, make the Nano tube array of titanium dioxide of 15-40nm diameter range, an anodic oxidation simultaneously and vibration back obtain circular nanoporous enlarged-diameter to 70-250nm, and circular port is transformed into the regular hexagon hole, thereby forms cellular orderly film of Nano tube array of titanium dioxide.
When two-step anodization voltage,, can control secondary oxidation and make titania nanotube length between 100-2000nm by changing oxidization time from 10-70min.
Claims (6)
1. cellular orderly film of Nano tube array of titanium dioxide is characterized in that:
Described cellular orderly titania nanotube shape array film is made up of upper and lower two-layer titanium dioxide nano-pore, and is supported on the titanium sheet substrate;
Described upper strata titanium dioxide nano-pore is orderly regular hexagon array, and its aperture is 70-250nm;
Described lower floor titanium dioxide nano-pore is real to be titania nanotube, and its opening end is to be arranged in the upper strata nanoporous, and each tube opening end is bonded to each other in the axial direction, and the aperture in lower floor hole is 15-40nm, and the degree of depth is 100-2000nm.
2. the preparation method of the described cellular orderly film of Nano tube array of titanium dioxide of a claim 1 is characterized in that may further comprise the steps:
(1) at first pure titanium sheet is put into that ultrasonic cleaning 55-65min removes the organism on surface in the mixing solutions of ethanol and acetone, and then cleaned repeatedly, and dry with deionized water;
(2) the titanium sheet after cleaning is dried is put into the ethylene glycol solution that contains 0.2mol/l hydrofluoric acid and is carried out anodic oxidation, and wherein oxidation voltage is 40-105v, and oxidization time is 1.2-1.5h, and titanium plate surface forms Nano tube array of titanium dioxide;
(3) will in hydrofluoric acid ethylene glycol ionogen, take out by anodised titanium sheet, place dehydrated alcohol, and, make the Nano tube array of titanium dioxide of titanium plate surface be removed by sonic oscillation, on titanium sheet substrate, stay the circular titanium dioxide nano-pore of ordered arrangement;
(4) preparation contains the ethylene glycol ionogen of 0.26mol/l Neutral ammonium fluoride, and will put into this ionogen through the titanium sheet after step (3) processing and carry out the anodic oxidation second time, its oxidation voltage is 15-30v, oxidization time is 10-70min, generate the more Nano tube array of titanium dioxide of minor diameter in the circular titanium dioxide nano-pore that this anode oxidation process can obtain in step (3), the circular titanium dioxide nano-pore enlarged-diameter of the middle acquisition of step (3) simultaneously, and circular port is transformed into the regular hexagon hole, thereby forms cellular orderly film of Nano tube array of titanium dioxide on the titanium sheet.
3. the preparation method of cellular orderly film of Nano tube array of titanium dioxide according to claim 2 is characterized in that: obtain by the twice electrochemical anodic oxidation processing in the ethylene glycol organic electrolyte solution of hydrofluoric acid containing, Neutral ammonium fluoride of titanium sheet.
4. the preparation method of cellular orderly Nano tube array of titanium dioxide according to claim 2, it is characterized in that: by changing an anodic oxidation voltage from 40v-105v, can make the Nano tube array of titanium dioxide of 50-120nm scope diameter, after the ultrasonic vibration processing, can obtain the titanium dioxide nano-pore array of diameter range at 60-180nm.
5. the preparation method of cellular orderly film of Nano tube array of titanium dioxide according to claim 2, it is characterized in that: during two-step anodization voltage, by changing oxidation voltage from 15-30v, can in the nanohole array after once oxidation is handled, make the Nano tube array of titanium dioxide of 15-40nm diameter range, an anodic oxidation simultaneously and vibration back obtain circular nanoporous enlarged-diameter to 70-250nm, and circular port is transformed into the regular hexagon hole, thereby forms cellular orderly film of Nano tube array of titanium dioxide.
6. the preparation method of cellular orderly film of Nano tube array of titanium dioxide according to claim 2, it is characterized in that: when two-step anodization voltage, by changing oxidization time, can control secondary oxidation and make titania nanotube length between 100-2000nm from 10-70min.
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| CN102418133A (en) * | 2011-12-12 | 2012-04-18 | 天津大学 | Nano honeycomb titanium dioxide structure thin film with rough surface and preparation method of nanohoneycomb titanium dioxide structure thin film |
| CN102489471A (en) * | 2011-12-20 | 2012-06-13 | 深圳市华测检测技术股份有限公司 | Method for cleaning sampling bottles |
| CN102674706A (en) * | 2012-06-01 | 2012-09-19 | 天津大学 | Method for preparing titanium dioxide nano multi-level structure thin film on conductive glass |
| CN102776543A (en) * | 2012-05-07 | 2012-11-14 | 中国科学院合肥物质科学研究院 | Preparation method of large-area smooth-surface uncracked anodic oxidation titanium dioxide nanometer tube arrays |
| CN103668389A (en) * | 2013-11-21 | 2014-03-26 | 中国科学院合肥物质科学研究院 | Preparation method of ultra-thin two-way titanium-dioxide nanopore-array film with adjustable aperture and thickness |
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| CN102418133B (en) * | 2011-12-12 | 2014-02-12 | 天津大学 | Nano honeycomb titanium dioxide structure thin film with rough surface and preparation method of nanohoneycomb titanium dioxide structure thin film |
| CN102418133A (en) * | 2011-12-12 | 2012-04-18 | 天津大学 | Nano honeycomb titanium dioxide structure thin film with rough surface and preparation method of nanohoneycomb titanium dioxide structure thin film |
| CN102489471A (en) * | 2011-12-20 | 2012-06-13 | 深圳市华测检测技术股份有限公司 | Method for cleaning sampling bottles |
| CN102776543A (en) * | 2012-05-07 | 2012-11-14 | 中国科学院合肥物质科学研究院 | Preparation method of large-area smooth-surface uncracked anodic oxidation titanium dioxide nanometer tube arrays |
| CN102776543B (en) * | 2012-05-07 | 2015-07-15 | 中国科学院合肥物质科学研究院 | Preparation method of large-area smooth-surface uncracked anodic oxidation titanium dioxide nanometer tube arrays |
| CN102674706A (en) * | 2012-06-01 | 2012-09-19 | 天津大学 | Method for preparing titanium dioxide nano multi-level structure thin film on conductive glass |
| CN103668389A (en) * | 2013-11-21 | 2014-03-26 | 中国科学院合肥物质科学研究院 | Preparation method of ultra-thin two-way titanium-dioxide nanopore-array film with adjustable aperture and thickness |
| CN103668389B (en) * | 2013-11-21 | 2016-05-11 | 中国科学院合肥物质科学研究院 | The preparation method of the ultra-thin bilateral titanium dioxide nano-pore array thin film that aperture and thickness are adjustable |
| CN103956269B (en) * | 2013-12-31 | 2018-02-06 | 湖北大学 | Growth in situ TiO2The preparation method of the DSSC of nano particle/nanotube |
| CN103956269A (en) * | 2013-12-31 | 2014-07-30 | 湖北大学 | Method for preparing dye-sensitized solar cell through in-situ growth of TiO2 nano-particles/nanotubes |
| CN104062321A (en) * | 2014-07-08 | 2014-09-24 | 苏州纳格光电科技有限公司 | Semiconductor gas sensor with gridding-shaped functional region |
| CN104707992A (en) * | 2014-12-01 | 2015-06-17 | 中国科学院合肥物质科学研究院 | Preparation method for superstructure Au/Ag@Al2O3@Ag nanosphere array and SERS performance of superstructure Au/Ag@Al2O3@Ag nanosphere array |
| CN105887157B (en) * | 2016-05-13 | 2017-05-31 | 中环清新人工环境工程技术(北京)有限责任公司 | A kind of preparation method that can be used for the cellular nano material of purification of air |
| CN105887157A (en) * | 2016-05-13 | 2016-08-24 | 中环清新人工环境工程技术(北京)有限责任公司 | Preparation method of honeycomb shaped nanometer material capable of purifying air |
| CN112064090A (en) * | 2020-09-16 | 2020-12-11 | 山东大学 | Microstructure surface preparation method with high blood compatibility and microstructure |
| CN112064090B (en) * | 2020-09-16 | 2022-02-08 | 山东大学 | Microstructure surface preparation method with high blood compatibility and microstructure |
| CN113481564A (en) * | 2021-06-30 | 2021-10-08 | 中国科学院金属研究所 | Titanium-based alloy with bionic super-smooth surface structure and preparation method and application thereof |
| CN114432500A (en) * | 2022-01-20 | 2022-05-06 | 南京医科大学附属口腔医院 | CeO (CeO)2Modified TiO2Bionic porous titanium stent of variable nanotube array and preparation method thereof |
| CN114432500B (en) * | 2022-01-20 | 2022-09-16 | 南京医科大学附属口腔医院 | CeO (CeO) 2 Modified TiO 2 2 Bionic porous titanium stent of variable nanotube array and preparation method thereof |
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