CN106044846A - Preparation method and application of nanorod self-assembled spike-like nano-ZnO - Google Patents

Preparation method and application of nanorod self-assembled spike-like nano-ZnO Download PDF

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Publication number
CN106044846A
CN106044846A CN201610402029.1A CN201610402029A CN106044846A CN 106044846 A CN106044846 A CN 106044846A CN 201610402029 A CN201610402029 A CN 201610402029A CN 106044846 A CN106044846 A CN 106044846A
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China
Prior art keywords
nano
zno
preparation
zine oxide
nano zine
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CN201610402029.1A
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CN106044846B (en
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杜建平
杜宇轩
高娜
何思源
郭天宇
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Taiyuan University of Technology
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Taiyuan University of Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00Compounds of zinc
    • C01G9/02Oxides; Hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004Gaseous mixtures, e.g. polluted air
    • G01N33/0009General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036Specially adapted to detect a particular component
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/45Aggregated particles or particles with an intergrown morphology

Abstract

This invention relates to the field of preparation of nano-ZnO, in particular to a preparation method and application of nanorod self-assembled spike-like nano-ZnO. Zinc nitrate and tetraethylammonium hydroxide are subjected to a reaction to synthesize nano-ZnO. The preparation method of nano-ZnO has the advantages that the raw materials adopted are easily available, the morphology is controllable, the product quality is stable, parameters are easy to control, the production cost is low, neither acid for treating the raw materials nor an organic solvent is required, the method belongs to a green synthesis technology and is simple, the production efficiency is high, the method is quite applicable to industrial production, can be used for detecting volatile organic compounds with low concentration, and can be particularly used for detecting propylene glycol; besides, nano-ZnO has the characteristics of high sensitivity and quick response compared with a conventional gas sensitive material.

Description

A kind of method preparing nanometer rods self assembly spike nano zine oxide and application thereof
Technical field
The present invention relates to the preparation field of nano zine oxide, specifically one, to prepare nanometer rods self assembly spike nano oxidized The method of zinc and application thereof.
Background technology
Performance and the application of nano material are had a great impact by structure and the pattern of nano material.Prepare ad hoc structure Nano material for exploitation nano ZnO frontier have important academic significance and using value.Receive numerous In rice material, the nanostructured of zinc oxide is of great interest.The zinc oxide of nanostructured is owing to having relatively Large ratio surface Long-pending and good magnetic, optical, electrical performance and attention, be expected to be applied to photocatalysis, gas sensor, moisture sensor, pressure-sensitive The various fields such as resistance, transparency electrode, has broad application prospects.
Therefore, work out and prepare the Nano-class zinc oxide preparation method of pattern cheap, simple to operate, novel and have important Scientific meaning.
Summary of the invention
It is desirable to provide a kind of method preparing nanometer rods self assembly spike nano zine oxide and application thereof.
The present invention is achieved by the following technical solutions: a kind of side preparing nanometer rods self assembly spike nano zine oxide Method, itself through the following steps that realize:
(1) zinc nitrate is dissolved in the water and forms the zinc nitrate solution of 40g~60g/L, is subsequently adding and zinc nitrate solution volume ratio It is the tetraethyl ammonium hydroxide of 9~11:50, stirs, form mixed solution;
(2) mixed solution in step (1) is transferred in reactor, at 105~115 DEG C of isothermal reaction 24h;
(3), after having reacted, room temperature is naturally cooled to, washing, it is dried to constant weight at 80 DEG C under air ambient, prepares nanometer rods Self assembly spike nano zine oxide.
Using zinc nitrate as zinc source in the present invention, zinc nitrate can ionize in the solution completely, provides for reaction and fills The zinc ion of foot, the zinc nitrate solution of 40g~60g/L ensure that and carries out under optimal alkali environment with tetraethyl ammonium hydroxide Reaction.Tetraethyl ammonium hydroxide serves main effect to the pattern of nano zine oxide.The zinc nitrate solution of 40g~60g/L With the pattern that the volume ratio of tetraethyl ammonium hydroxide, preparation parameter (temperature, time) have together decided on nano zine oxide.
It addition, the nanometer rods self assembly spike nano zine oxide that the present invention prepares makes gas sensor in detection volatilization Application in property Organic substance.
Relative to prior art, the present invention has the advantages that preparation method is raw materials used and is easy to get, morphology controllable, The steady quality of product, each parameter is easily controllable, and production cost is low, both need not use acid treatment raw material, it is not required that uses and has Machine solvent, belongs to green synthesis techniques, and method is easy, and production efficiency is high, and pole is applicable to industrialized production, can be used for detecting low dense Degree volatile organic matter, especially propylene glycol, relative to conventional gas sensitive, have susceptiveness height, respond fast feature.
Test: the zinc oxide of the present invention sensitivity tests to various gases
The second of 1.1 300ppm that the gas sensor that nanometer rods self assembly spike nano zine oxide is made is respectively placed in 300 DEG C Under the atmosphere of alcohol, methanol, ethylene glycol, propylene glycol, benzene, dimethylbenzene, acetone and formaldehyde, carry out gas sensitization performance test, find The nanometer rods self assembly spike nano zine oxide that the present invention the prepares selectivity the highest (seeing Fig. 2) to propylene glycol.
Again the gas sensor that nanometer rods self assembly spike nano zine oxide is made is placed in 300 DEG C 5ppm, 30ppm, In the propylene glycol gas of 100ppm, 200ppm and 300ppm, the response value of result display propylene glycol is respectively 27,75,87,90 Fig. 3 is seen) with 94(.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the nanometer rods self assembly spike nano zine oxide that the present invention prepares.Dark color in figure Region part is partial enlarged drawing.
Fig. 2 is that the gas sensor made of the nanometer rods self assembly spike nano zine oxide that the present invention prepares is to various gas The sensitive property test result comparison diagram of body.
Fig. 3 is that the gas sensor that the nanometer rods self assembly spike nano zine oxide that the present invention prepares is made is dense to difference The response value comparison diagram of degree propylene glycol gas.
Detailed description of the invention
Embodiment 1
A kind of method preparing nanometer rods self assembly spike nano zine oxide, itself through the following steps that realize:
(1) 2g zinc nitrate is dissolved in 50ml water formation zinc nitrate solution, is subsequently adding the tetraethyl ammonium hydroxide of 9ml, stirs Mix uniformly, form mixed solution;
(2) mixed solution in step (1) is transferred in reactor, at 105 DEG C of isothermal reaction 24h;
(3), after having reacted, room temperature is naturally cooled to, washing, it is dried to constant weight at 80 DEG C under air ambient, prepares nanometer rods Self assembly spike nano zine oxide.
Embodiment 2
A kind of method preparing nanometer rods self assembly spike nano zine oxide, itself through the following steps that realize:
(1) 3g zinc nitrate is dissolved in 50ml water formation zinc nitrate solution, is subsequently adding the tetraethyl ammonium hydroxide of 11ml, stirs Mix uniformly, form mixed solution;
(2) mixed solution in step (1) is transferred in reactor, at 115 DEG C of isothermal reaction 24h;
(3), after having reacted, room temperature is naturally cooled to, washing, it is dried to constant weight at 80 DEG C under air ambient, prepares nanometer rods Self assembly spike nano zine oxide.
Embodiment 3
A kind of method preparing nanometer rods self assembly spike nano zine oxide, itself through the following steps that realize:
(1) 2.5g zinc nitrate is dissolved in 50ml water formation zinc nitrate solution, is subsequently adding the tetraethyl ammonium hydroxide of 10ml, Stir, form mixed solution;
(2) mixed solution in step (1) is transferred in reactor, at 112 DEG C of isothermal reaction 24h;
(3), after having reacted, room temperature is naturally cooled to, washing, it is dried to constant weight at 80 DEG C under air ambient, prepares nanometer rods Self assembly spike nano zine oxide.

Claims (2)

1. the method preparing nanometer rods self assembly spike nano zine oxide, it is characterised in that it is through the following steps that real Existing:
(1) zinc nitrate is dissolved in the water and forms the zinc nitrate solution of 40g~60g/L, is subsequently adding and zinc nitrate solution volume ratio It is the tetraethyl ammonium hydroxide of 9~11:50, stirs, form mixed solution;
(2) mixed solution in step (1) is transferred in reactor, at 105~115 DEG C of isothermal reaction 24h;
(3), after having reacted, room temperature is naturally cooled to, washing, it is dried to constant weight at 80 DEG C under air ambient, prepares nanometer rods Self assembly spike nano zine oxide.
2. the nanometer rods self assembly spike nano zine oxide that claim 1 prepares makes gas sensor to be had in detection volatility Application in machine thing.
CN201610402029.1A 2016-06-08 2016-06-08 A kind of method and its application for preparing nanometer rods self assembly spike nano zine oxide Active CN106044846B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103101964A (en) * 2013-01-16 2013-05-15 浙江大学 Preparation method of zinc oxide nanoflower of spiauterite structure
CN103586013A (en) * 2013-11-13 2014-02-19 河北师范大学 Method for preparing wheat-ear-shaped nano ZnO photocatalyst

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103101964A (en) * 2013-01-16 2013-05-15 浙江大学 Preparation method of zinc oxide nanoflower of spiauterite structure
CN103586013A (en) * 2013-11-13 2014-02-19 河北师范大学 Method for preparing wheat-ear-shaped nano ZnO photocatalyst

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
刘领等: "季铵碱水溶液中微波辅助制备纳米ZnO", 《厦门大学学报》 *
陈庆春等: "纳米花形氧化锌颗粒的水热制备", 《中国颗粒学会2006年年会暨海峡两岸颗粒技术研讨会》 *
黄开金: "《纳米材料的制备与应用》", 30 April 2009, 冶金工业出版社 *

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