CN107961805A - The TiO of N doping2The preparation method of nano-wire array - Google Patents

The TiO of N doping2The preparation method of nano-wire array Download PDF

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Publication number
CN107961805A
CN107961805A CN201610911325.4A CN201610911325A CN107961805A CN 107961805 A CN107961805 A CN 107961805A CN 201610911325 A CN201610911325 A CN 201610911325A CN 107961805 A CN107961805 A CN 107961805A
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Prior art keywords
tio
nano
wire array
doping
preparation
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CN201610911325.4A
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Chinese (zh)
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丁磊
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Zhangjagang City Sha Yuan Detection Technique Co Ltd
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Zhangjagang City Sha Yuan Detection Technique Co Ltd
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Priority to CN201610911325.4A priority Critical patent/CN107961805A/en
Publication of CN107961805A publication Critical patent/CN107961805A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24Nitrogen compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of TiO of N doping2The preparation method of nano-wire array, including:S1, by TiO2After powder, surfactant are mixed with aqueous slkali, it is placed in autoclave, 1~24h of hydro-thermal reaction is carried out at 200~250 DEG C;Autoclave, is cooled to 20 DEG C by S2, and solid reactant therein is washed with ethanol and deionized water successively and removes surfactant, adjusts pH to 6~8, then removing chlorion is washed with deionized, and TiO is obtained after drying2Nano-wire array;S3, by TiO2Nano-wire array is positioned in tube furnace, and ammonium hydroxide is passed through into tube furnace, and heating makes ammonium hydroxide volatilize, with TiO2N doping is carried out in nano-wire array, obtains the TiO of N doping2Nano-wire array.The present invention can quickly prepare caliber, pipe range and the adjustable one-dimensional TiO of wall thickness2Nano wire;The one-dimensional TiO of nitrogen modification2Nano wire possesses the carrier transport ability of higher, so as to improve photocatalysis performance.

Description

The TiO of N doping2The preparation method of nano-wire array
Technical field
The present invention relates to semiconductor light-catalyst technical field, more particularly to a kind of TiO of N doping2Nano-wire array Preparation method.
Background technology
With expanding economy, water pollution situation is serious all the more, and photocatalysis technology is at waste water developed in recent years Reason technology.Photochemical catalyst is the material for causing catalytic reaction under light irradiation, and by light-catalyzed reaction, generation has Strong oxdiative ability Hydroxyl radical free radical and super oxonium ion, come decomposing organic pollutant matter of degrading.
Titanium dioxide (TiO2) it is a kind of most extensive semiconductor light-catalyst, it is widely used in photocatalysis field. But TiO2Greater band gap, can only show photochemical activity in ultra-violet (UV) band of the wavelength less than 378nm, while its photoelectron and hole hold Easily occur it is compound, so as to reduce photocatalysis efficiency.
TiO2Nano material such as nano wire, nanotube, can be with than the surface area and volume ratio that common nanoparticle has higher Of a relatively high avtive spot density is provided, be conducive to surface reaction occur and sensitizer load, and one-dimensional make its Photo-generated carrier is separated possesses faster charge carrier transport speed with transfer device application.Also just because of these are excellent Gesture, nano-TiO2Synthesis obtain it is continual concern and break through, this has also pushed directly on TiO2The extensive use of material. Divided according to Spatial Dimension, TiO2Nano material can simply be divided into one-dimensional, two and three dimensions nano material, wherein one-dimentional structure More it is widely applied.
Therefore, in view of the above-mentioned problems, being necessary to propose a kind of TiO of N doping2The preparation method of nano-wire array.
The content of the invention
In view of this, the present invention provides a kind of TiO of N doping2The preparation method of nano-wire array.
In order to realize foregoing invention purpose, the present invention provides a kind of TiO of N doping2The preparation method of nano-wire array, The preparation method includes:
S1, by TiO2After powder, surfactant are mixed with aqueous slkali, be placed in autoclave, at 200~250 DEG C into 1~24h of row hydro-thermal reaction;
Autoclave, is cooled to 20 DEG C by S2, and solid reactant therein is washed removing with ethanol and deionized water successively Surfactant, adjusts pH to 6~8, then removing chlorion is washed with deionized, and TiO is obtained after drying2Nano-wire array;
S3, by TiO2Nano-wire array is positioned in tube furnace, and ammonium hydroxide is passed through into tube furnace, and heating waves ammonium hydroxide Hair, with TiO2N doping is carried out in nano-wire array, obtains the TiO of N doping2Nano-wire array.
As a further improvement on the present invention, aqueous slkali is KOH or NaOH solution in the step S1, concentration for 1~ 10M。
As a further improvement on the present invention, TiO in the step S12The dosage of powder, surfactant and aqueous slkali Than for 0.5~1g:2~4g:1~50mL.
As a further improvement on the present invention, the step S1 mesohigh kettles hydrothermal temperature is 220 DEG C, the reaction time For 20h.
As a further improvement on the present invention, the temperature of N doping is 400 DEG C in the step S3, doping time 5h.
Compared with prior art, the beneficial effects of the invention are as follows:
The present invention can quickly prepare caliber, pipe range and the adjustable one-dimensional TiO of wall thickness2Nano wire;Nitrogen is modified one-dimensional TiO2Nano wire possesses the carrier transport ability of higher, so as to improve photocatalysis performance.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing There is attached drawing needed in technology description to be briefly described, it should be apparent that, drawings in the following description are only this Some embodiments described in invention, for those of ordinary skill in the art, without creative efforts, Other attached drawings can also be obtained according to these attached drawings.
Fig. 1 is the TiO of N doping in the present invention2The flow diagram of the preparation method of nano-wire array.
Embodiment
The technical solution in the embodiment of the present invention will be described in detail below, it is clear that described embodiment is only Only it is part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill Personnel's all other embodiments obtained on the premise of creative work is not made, belong to the model that the present invention protects Enclose.
Join shown in Fig. 1, a kind of TiO of N doping in the present invention2The preparation method of nano-wire array, specifically includes:
S1, by TiO2After powder, surfactant are mixed with aqueous slkali, be placed in autoclave, at 200~250 DEG C into 1~24h of row hydro-thermal reaction;
Autoclave, is cooled to 20 DEG C by S2, and solid reactant therein is washed removing with ethanol and deionized water successively Surfactant, adjusts pH to 6~8, then removing chlorion is washed with deionized, and TiO is obtained after drying2Nano-wire array;
S3, by TiO2Nano-wire array is positioned in tube furnace, and ammonium hydroxide is passed through into tube furnace, and heating waves ammonium hydroxide Hair, with TiO2N doping is carried out in nano-wire array, obtains the TiO of N doping2Nano-wire array.
Specifically, in a preferred embodiment, the TiO of N doping2The preparation method of nano-wire array, specific bag Include:
S1, by TiO2After powder, surfactant are mixed with aqueous slkali, be placed in autoclave, at 200~250 DEG C into Row 1~24h of hydro-thermal reaction, wherein, aqueous slkali is KOH or NaOH solution, and concentration is 1~10M;TiO2Powder, surfactant Amount ratio with aqueous slkali is 0.5~1g:2~4g:1~50mL;Autoclave hydrothermal temperature is 220 DEG C, and the reaction time is 20h;
Autoclave, is cooled to 20 DEG C by S2, and solid reactant therein is washed removing with ethanol and deionized water successively Surfactant, adjusts pH to 6~8, then removing chlorion is washed with deionized, and TiO is obtained after drying2Nano-wire array;
S3, by TiO2Nano-wire array is positioned in tube furnace, and ammonium hydroxide is passed through into tube furnace, and heating waves ammonium hydroxide Hair, with TiO2N doping is carried out in nano-wire array, the temperature of N doping is 400 DEG C, and doping time 5h, obtains N doping TiO2Nano-wire array.
As can be seen from the above technical solutions, it is adjustable one-dimensional can quickly to prepare caliber, pipe range and wall thickness by the present invention TiO2Nano wire;The one-dimensional TiO of nitrogen modification2Nano wire possesses the carrier transport ability of higher, so as to improve photocatalysis performance.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling Change is included in the present invention.Any reference numeral in claim should not be considered as to the involved claim of limitation.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped Containing an independent technical solution, this narrating mode of specification is only that those skilled in the art should for clarity Using specification as an entirety, the technical solution in each embodiment can also be closed through appropriate, and forming those skilled in the art can With the other embodiment of understanding.

Claims (5)

  1. A kind of 1. TiO of N doping2The preparation method of nano-wire array, it is characterised in that the preparation method includes:
    S1, by TiO2After powder, surfactant are mixed with aqueous slkali, it is placed in autoclave, hydro-thermal is carried out at 200~250 DEG C React 1~24h;
    Autoclave, is cooled to 20 DEG C by S2, and solid reactant therein is washed with ethanol and deionized water successively and removes surface Activating agent, adjusts pH to 6~8, then removing chlorion is washed with deionized, and TiO is obtained after drying2Nano-wire array;
    S3, by TiO2Nano-wire array is positioned in tube furnace, and ammonium hydroxide is passed through into tube furnace, heating ammonium hydroxide is volatilized, with TiO2N doping is carried out in nano-wire array, obtains the TiO of N doping2Nano-wire array.
  2. 2. preparation method according to claim 1, it is characterised in that aqueous slkali is molten for KOH or NaOH in the step S1 Liquid, concentration are 1~10M.
  3. 3. preparation method according to claim 2, it is characterised in that TiO in the step S12Powder, surfactant with The amount ratio of aqueous slkali is 0.5~1g:2~4g:1~50mL.
  4. 4. preparation method according to claim 1, it is characterised in that the step S1 mesohighs kettle hydrothermal temperature is 220 DEG C, reaction time 20h.
  5. 5. preparation method according to claim 1, it is characterised in that the temperature of N doping is 400 DEG C in the step S3, Doping time is 5h.
CN201610911325.4A 2016-10-20 2016-10-20 The TiO of N doping2The preparation method of nano-wire array Pending CN107961805A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101279250A (en) * 2008-02-01 2008-10-08 浙江大学 Load type nitrogen intermingle with one-dimensional structure TiO2 and preparation method thereof
CN101814375A (en) * 2009-02-25 2010-08-25 清华大学 Preparation method of nitrogen-doped titanium dioxide nano line electrode
CN102826600A (en) * 2012-09-20 2012-12-19 电子科技大学 Method for preparing titanium dioxide nanowire
CN104001504A (en) * 2014-05-13 2014-08-27 河海大学 Preparation method for silver and graphene co-modified TiO2 nanowire and application of silver and graphene co-modified TiO2 nanowire in photocatalytic degradation of pollutants in waste water

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101279250A (en) * 2008-02-01 2008-10-08 浙江大学 Load type nitrogen intermingle with one-dimensional structure TiO2 and preparation method thereof
CN101814375A (en) * 2009-02-25 2010-08-25 清华大学 Preparation method of nitrogen-doped titanium dioxide nano line electrode
CN102826600A (en) * 2012-09-20 2012-12-19 电子科技大学 Method for preparing titanium dioxide nanowire
CN104001504A (en) * 2014-05-13 2014-08-27 河海大学 Preparation method for silver and graphene co-modified TiO2 nanowire and application of silver and graphene co-modified TiO2 nanowire in photocatalytic degradation of pollutants in waste water

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
JIN WANG, ET AL: "Origin of Photocatalytic Activity of Nitrogen-Doped TiO2 Nanobelts", 《J. AM. CHEM. SOC.》 *
MING-CHUNG WU, ET AL: "Nitrogen-Doped Anatase Nanofibers Decorated with Noble Metal Nanoparticles for Photocatalytic Production of Hydrogen", 《ACSNANO》 *
SIRIPHAN CHAINARONG, ET AL: "Synthesis and Characterization of Nitrogen-doped TiO2", 《ENERGY PROCEDIA》 *

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