CN107978458A - ZnO nanorod/TiO2The preparation method of nanoparticle composite film - Google Patents

ZnO nanorod/TiO2The preparation method of nanoparticle composite film Download PDF

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Publication number
CN107978458A
CN107978458A CN201610919961.1A CN201610919961A CN107978458A CN 107978458 A CN107978458 A CN 107978458A CN 201610919961 A CN201610919961 A CN 201610919961A CN 107978458 A CN107978458 A CN 107978458A
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China
Prior art keywords
tio
zno nanorod
composite film
preparation
nanoparticle composite
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CN201610919961.1A
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Chinese (zh)
Inventor
陈品良
常玲
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Jiangsu Dao Dao Investment Development Co Ltd
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Jiangsu Dao Dao Investment Development Co Ltd
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Priority to CN201610919961.1A priority Critical patent/CN107978458A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/20Light-sensitive devices
    • H01G9/2027Light-sensitive devices comprising an oxide semiconductor electrode
    • H01G9/2031Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/20Light-sensitive devices
    • H01G9/2027Light-sensitive devices comprising an oxide semiconductor electrode
    • H01G9/204Light-sensitive devices comprising an oxide semiconductor electrode comprising zinc oxides, e.g. ZnO
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/542Dye sensitized solar cells

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Hybrid Cells (AREA)

Abstract

The invention discloses a kind of ZnO nanorod/TiO2The preparation method of nanoparticle composite film, including:S1, by ammonia spirit add TiCl4With in the mixed solution of ethanol, and being stirred under magnetic fields, presoma is obtained;S2, by presoma by centrifugation after, cleaned using ultrasound, and dried;S3, calcine 1~5h under the conditions of 200~300 DEG C, obtains TiO2Nano particle;S4, reacted by low-temperature hydrothermal, in TiO2Growing ZnO nanorod in the hole of nanometer particle film, obtains ZnO nanorod/TiO2Nanoparticle composite film.ZnO nanorod/TiO of the present invention2Nanoparticle composite film can be widely applied to the technical fields such as dye-sensitized solar cells, can significantly improve photoelectric conversion efficiency.

Description

ZnO nanorod/TiO2The preparation method of nanoparticle composite film
Technical field
The present invention relates to semiconductor light-catalyst technical field, more particularly to a kind of ZnO nanorod/TiO2Nano particle The preparation method of laminated film.
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.
By TiO2Laminated film prepared by nano particle can be widely applied to the technical fields such as dye-sensitized solar cells, But its photoelectric conversion efficiency is generally relatively low.
Therefore, in view of the above-mentioned problems, being necessary to propose a kind of ZnO nanorod //TiO2The preparation of nanoparticle composite film Method.
The content of the invention
In view of this, the present invention provides a kind of ZnO nanorod/TiO2The preparation method of nanoparticle composite film.
In order to realize foregoing invention purpose, the present invention provides a kind of ZnO nanorod/TiO2The system of nanoparticle composite film Preparation Method, the preparation method include:
S1, by ammonia spirit add TiCl4With in the mixed solution of ethanol, and being stirred under magnetic fields, forerunner is obtained Body;
S2, by presoma by centrifugation after, cleaned using ultrasound, and dried;
S3, calcine 1~5h under the conditions of 200~300 DEG C, obtains TiO2Nano particle;
S4, reacted by low-temperature hydrothermal, in TiO2Growing ZnO nanorod in the hole of nanometer particle film, obtains ZnO and receives Rice rod/TiO2Nanoparticle composite film.
As a further improvement on the present invention, TiCl in the mixed solution of the step S14With ethanol mole the ratio between be 1:50~1:100.
As a further improvement on the present invention, calcining heat is 250 DEG C in the step S2, calcination time 4h.
As a further improvement on the present invention, the solution that low-temperature hydrothermal reaction uses in the step S3 is Zn (NO3)2Water Solution, reaction temperature are 70~90 DEG C, and the reaction time is 15~25h.
Compared with prior art, the beneficial effects of the invention are as follows:
ZnO nanorod/TiO of the present invention2Nanoparticle composite film, can both retain TiO2Nano particle specific surface area The advantages of big and electron injection efficiency is high, and TiO can be made up2Nanoparticle three-dimensional net structure electrons spread transmission rate is slow The shortcomings that, the technical fields such as dye-sensitized solar cells are can be widely applied to, photoelectric conversion efficiency can be significantly improved.
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 ZnO nanorod/TiO in the present invention2The flow diagram of the preparation method of nanoparticle composite film.
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 ZnO nanorod/TiO in the present invention2The preparation method of nanoparticle composite film, including:
S1, by ammonia spirit add TiCl4With in the mixed solution of ethanol, and being stirred under magnetic fields, forerunner is obtained Body;
S2, by presoma by centrifugation after, cleaned using ultrasound, and dried;
S3, calcine 1~5h under the conditions of 200~300 DEG C, obtains TiO2Nano particle;
S4, reacted by low-temperature hydrothermal, in TiO2Growing ZnO nanorod in the hole of nanometer particle film, obtains ZnO and receives Rice rod/TiO2Nanoparticle composite film.
Specifically, in a preferred embodiment, a kind of ZnO nanorod/TiO2The system of nanoparticle composite film Preparation Method, including:
S1, by ammonia spirit add TiCl4With in the mixed solution of ethanol, wherein, TiCl4With ethanol mole the ratio between be 1:50~1:100, and stirred under magnetic fields, obtain presoma;
S2, by presoma by centrifugation after, cleaned using ultrasound, and dried;
S3, calcine 4h under the conditions of 250 DEG C, obtains TiO2Nano particle;
S4, reacted by low-temperature hydrothermal, and the solution that low-temperature hydrothermal reaction uses is Zn (NO3)2Aqueous solution, reaction temperature are 70~90 DEG C, the reaction time is 15~25h, in TiO2Growing ZnO nanorod in the hole of nanometer particle film, obtains ZnO and receives Rice rod/TiO2Nanoparticle composite film.
As can be seen from the above technical solutions, ZnO nanorod/TiO of the invention2Nanoparticle composite film, both can be with Retain TiO2The advantages of nano particle specific surface area is greatly and electron injection efficiency is high, and TiO can be made up2Nanoparticle three-dimensional net The shortcomings that shape structure electrical diffusion transport speed is slow, can be widely applied to the technical fields such as dye-sensitized solar cells, can Significantly improve photoelectric conversion efficiency.
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 (4)

  1. A kind of 1. ZnO nanorod/TiO2The preparation method of nanoparticle composite film, it is characterised in that the preparation method bag Include:
    S1, by ammonia spirit add TiCl4With in the mixed solution of ethanol, and being stirred under magnetic fields, presoma is obtained;
    S2, by presoma by centrifugation after, cleaned using ultrasound, and dried;
    S3, calcine 1~5h under the conditions of 200~300 DEG C, obtains TiO2Nano particle;
    S4, reacted by low-temperature hydrothermal, in TiO2Growing ZnO nanorod in the hole of nanometer particle film, acquisition ZnO nanorod/ TiO2Nanoparticle composite film.
  2. 2. preparation method according to claim 1, it is characterised in that TiCl in the mixed solution of the step S14With ethanol Mole the ratio between be 1:50~1:100.
  3. 3. preparation method according to claim 1, it is characterised in that calcining heat is 250 DEG C in the step S2, calcining Time is 4h.
  4. 4. preparation method according to claim 1, it is characterised in that low-temperature hydrothermal reaction uses molten in the step S3 Liquid is Zn (NO3)2Aqueous solution, reaction temperature are 70~90 DEG C, and the reaction time is 15~25h.
CN201610919961.1A 2016-10-21 2016-10-21 ZnO nanorod/TiO2The preparation method of nanoparticle composite film Pending CN107978458A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101966450A (en) * 2010-07-29 2011-02-09 中国计量学院 High-efficiency composite photocatalyst and preparation method thereof
CN102254704A (en) * 2011-05-06 2011-11-23 海南科技职业学院 Dye sensitized noble metal deposited titanium dioxide light anode and preparation method thereof
CN102658112A (en) * 2012-04-14 2012-09-12 黑龙江省金昇新能源与环境材料研究院 Preparation method of ZnO-TiO2 composite photocatalyst
CN103456511A (en) * 2012-06-04 2013-12-18 中国石油大学(华东) Post-embedding method for preparing ZnO nanorod/TiO2 nano-particle composite film
CN104952963A (en) * 2015-04-14 2015-09-30 上海大学 Method for preparing TiO2-ZnO hetero-junction nanorod for perovskite solar cell

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101966450A (en) * 2010-07-29 2011-02-09 中国计量学院 High-efficiency composite photocatalyst and preparation method thereof
CN102254704A (en) * 2011-05-06 2011-11-23 海南科技职业学院 Dye sensitized noble metal deposited titanium dioxide light anode and preparation method thereof
CN102658112A (en) * 2012-04-14 2012-09-12 黑龙江省金昇新能源与环境材料研究院 Preparation method of ZnO-TiO2 composite photocatalyst
CN103456511A (en) * 2012-06-04 2013-12-18 中国石油大学(华东) Post-embedding method for preparing ZnO nanorod/TiO2 nano-particle composite film
CN104952963A (en) * 2015-04-14 2015-09-30 上海大学 Method for preparing TiO2-ZnO hetero-junction nanorod for perovskite solar cell

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Application publication date: 20180501