CN103803635A - Preparation method of Li ion-doped ZnO superfine nano rod - Google Patents
Preparation method of Li ion-doped ZnO superfine nano rod Download PDFInfo
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- CN103803635A CN103803635A CN201410067705.5A CN201410067705A CN103803635A CN 103803635 A CN103803635 A CN 103803635A CN 201410067705 A CN201410067705 A CN 201410067705A CN 103803635 A CN103803635 A CN 103803635A
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Abstract
The invention discloses a preparation method of a Li ion-doped ZnO superfine nano rod with lower cost. The preparation method comprises the following steps: 1, mixing fatty acid zinc, fatty acid lithium and 1-octadecene and uniformly stirring in a reaction flask by a magnetic force, heating to 100-150 DEG C, then vacuumizing to remove water vapor and oxygen in a reaction system, then heating to 200-300 DEG C under an inert gas protection atmosphere; 2, injecting stearyl alcohol at a temperature of 100-200 DEG C and 1-octadecene in the reaction flask, insulating for 1-100 minutes, and cooling to a room temperature; 3, centrifugally separating a reaction mixture in the reaction flask to obtain the Li ion-doped ZnO superfine nano rod. The preparation method has the advantages of simple process, lower cost, good controllability, and availability in industrialized production; the prepared Li ion-doped ZnO superfine nano rod has a hexagonal wurtzite structure with the diameter of a nano wire is 3-10nm and a length of 10-20nm, and is expected to be applied in multiple fields such as blue-violet light-emitting diodes and gas sensors.
Description
Technical field
The present invention relates to technical field of nano material, be specifically related to a kind of preparation method of Li doped ion Zn O superfine nano rod.
Background technology
ZnO is a kind of direct band-gap semicondictor material, under room temperature, energy gap is 3.37eV, exciton bind energy is 60meV, energy gap is large, electronic drift saturating speed is high, specific inductivity is little and have excellent photoelectric characteristic, can be widely used in the numerous areas such as transparency electrode, piezoelectricity conversion, surface acoustic wave device, pressure-sensitive sensing element, wet sensitive, gas sensor and solar cell.Optical, electrical and the magnetic behavior that is better than other structures that ZnO monodimension nanometer material has due to quantum confined effect, surface effects, piezoelectric effect etc. etc. has become the focus of current research.Device based on this nanostructure provides effective solution for the problem that solves the aspects such as the energy, environment, biology, electronics, photoelectricity as nano generator, nano field-effect transistor, nano-sensor, nano solar battery etc.The method of the ZnO one dimension Nano structure of synthesizing blender Li mainly contains pulsed laser deposition, thermal evaporation, metal organic chemical vapor deposition, sol-gel method, hydrothermal method etc. at present.These preparation methods' main deficiency is that apparatus expensive or complex process, poor controllability, doping are inhomogeneous etc., and the diameter of the Li doping zinc oxide nanometer rod obtaining is generally more than tens nanometers, and this has limited its application in field of nanometer devices widely.
Summary of the invention
Technical problem to be solved by this invention is: the preparation method that a kind of lower-cost Li doped ion Zn O superfine nano rod is provided.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: the preparation method of Li doped ion Zn O superfine nano rod, comprise the steps: 1) fatty acid zinc, fatty acid lithium and 1-octadecylene are mixed to be placed in reaction flask magnetic agitation even, be warming up to after 100～150 ℃ and vacuumize water vapor and the oxygen removed in reaction system, then under protection of inert gas atmosphere, be heated to 200～300 ℃;
2) be that stearyl alcohol and the 1-octadecylene of 100～200 ℃ is injected in reaction flask by temperature, insulation 1～100 min, is cooled to room temperature;
3), by the reaction mixture centrifugation in reaction flask, obtain Li doped ion Zn O superfine nano rod.
In order to solve the problems of the technologies described above better, the further technical scheme that the present invention adopts is: described rare gas element is that purity is more than 99.99% argon gas or nitrogen.
Advantage of the present invention is: the preparation method of Li doped ion Zn O superfine nano rod, technique is simple, cost is lower, controllability good, be easy to suitability for industrialized production, the Li doped ion Zn O superfine nano rod obtaining there is hexagonal wurtzite structure, the diameter of nano wire is 3～10nm, length is 10～20nm, is expected to be applied at numerous areas such as royal purple light-emitting diode, gas sensors.
Accompanying drawing explanation
Fig. 1 is that preparation method Fig. 1 lithium stearate of Li doped ion Zn O superfine nano rod of the present invention and the mol ratio of Zinic stearas are (a) 0: 1, (b) 1: 9, (c) 3: 7, (d) XRD figure of 1: 1 o'clock gained sample.
The mol ratio of Fig. 2 lithium stearate and Zinic stearas is (a) 0: 1, (b) 1: 9, and (c) 3: 7, (d) the TEM figure of 1: 1 o'clock gained sample.
The mol ratio of Fig. 3 lithium stearate and Zinic stearas is (a) 0: 1, (b) 1: 9, and (c) 3: 7, (d) photoluminescence of 1: 1 o'clock gained sample (PL) figure.
Embodiment
Describe in detail particular content of the present invention below by the drawings and specific embodiments.
The preparation method of Li doped ion Zn O superfine nano rod, comprise the steps: 1) fatty acid zinc, fatty acid lithium and 1-octadecylene are mixed to be placed in reaction flask magnetic agitation even, be warming up to after 100～150 ℃ and vacuumize water vapor and the oxygen removed in reaction system, then under protection of inert gas atmosphere, be heated to 200～300 ℃;
2) be that stearyl alcohol and the 1-octadecylene of 100～200 ℃ is injected in reaction flask by temperature, insulation 1～100 min, is cooled to room temperature;
3), by the reaction mixture centrifugation in reaction flask, obtain Li doped ion Zn O superfine nano rod.
Described rare gas element is that purity is more than 99.99% argon gas or nitrogen.
Embodiment 1
1) take 0.01452g lithium stearate, 0.2844g Zinic stearas (mol ratio is 1: 9) and 10g1-octadecylene and be placed in 50ml reaction flask; under magnetic agitation, be warming up to 100 ℃; then reaction flask is vacuumized to 20min; to remove water vapor and the oxygen in reaction system, be, under the protective atmosphere of 99.99% nitrogen, reaction soln is warming up to rapidly to 200 ℃ in purity.
2) the 0.676g stearyl alcohol and the 2.5g1-octadecylene that are 160 ℃ temperature are injected in reaction flask rapidly, and are incubated 20min, and question response solution is cooled to room temperature;
3) by the reaction mixture centrifugation in reaction flask, acquisition diameter is 5～7nm, the ZnO nanorod of the Li doping that length is 15～20nm.
Embodiment 2
1) take 0.04356g lithium stearate, 0.2212g Zinic stearas (mol ratio is 3: 7) and 10g1-octadecylene and be placed in 50ml reaction flask, under magnetic agitation, be warming up to 120 ℃, then reaction flask is vacuumized to 20 min, to remove water vapor and the oxygen in reaction system.Be, under the protective atmosphere of 99.99% argon gas, reaction soln is warming up to rapidly to 290 ℃ in purity;
2) the 0.676g stearyl alcohol and the 2.5g1-octadecylene that are 180 ℃ temperature are injected in reaction flask rapidly, and are incubated 20min, are cooled to room temperature;
3) by the reaction mixture centrifugation in reaction flask, acquisition diameter is 3～5nm, the ZnO nanorod of the Li doping that length is 15～20nm.
Embodiment 3
1) take 0.0726 g lithium stearate, 0.158 g Zinic stearas (mol ratio is 1: 1) and 10g1-octadecylene and be placed in 100ml reaction flask, under magnetic agitation, be warming up to 150 ℃, then reaction flask is vacuumized to 20 min, to remove water vapor and the oxygen in reaction system.Be, under the protective atmosphere of 99.99% nitrogen, reaction soln is warming up to rapidly to 270 ℃ in purity;
2) the 0.676g stearyl alcohol and the 2.5g1-octadecylene that are 200 ℃ temperature are injected in reaction flask rapidly, and are incubated 20 min, are cooled to room temperature;
3) by the reaction mixture centrifugation in reaction flask, the ZnO nanorod of the Li doping that acquisition 3～5nm, length are 10～15nm.
After the white product obtaining is dry, carry out XRD test, test result is shown in Fig. 1.Peak in Fig. 1 is all the main peak position of wurtzite ZnO phase, proves that the product obtaining is wurtzite structure.The TEM electromicroscopic photograph of product is shown in Fig. 2, and as can be seen from the figure, while doping, ZnO is triangular pyramidal, and the diameter of the superfine nano rod obtaining after Li doped is that 3～10nm, length are 10～20nm.The PL spectrogram of product is shown in Fig. 3, and as can be seen from the figure, the UV peak red shift of the rear ZnO of Li doping is to royal purple light district, and the peak, visible region being caused by defect strengthens.
Claims (2)
1. the preparation method of Li doped ion Zn O superfine nano rod, it is characterized in that: comprise the steps: 1) fatty acid zinc, fatty acid lithium and 1-octadecylene are mixed to be placed in reaction flask magnetic agitation even, be warming up to after 100～150 ℃ and vacuumize water vapor and the oxygen removed in reaction system, then under protection of inert gas atmosphere, be heated to 200～300 ℃;
2) be that stearyl alcohol and the 1-octadecylene of 100～200 ℃ is injected in reaction flask by temperature, insulation 1～100 min, is cooled to room temperature;
3), by the reaction mixture centrifugation in reaction flask, obtain Li doped ion Zn O superfine nano rod.
2. according to the preparation method of Li doped ion Zn O superfine nano rod claimed in claim 1, it is characterized in that: described rare gas element is that purity is more than 99.99% argon gas or nitrogen.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108821327A (en) * | 2018-06-27 | 2018-11-16 | 五邑大学 | The preparation method and its application of the pineal ZnO nano microballoon of one type |
| WO2023169017A1 (en) * | 2022-03-07 | 2023-09-14 | 深圳先进技术研究院 | Zinc oxide nanorod array photo-anode and preparation method therefor |
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| CN101445961A (en) * | 2008-12-15 | 2009-06-03 | 浙江大学 | Superfine Mg-doped ZnO nano wire and synthetic method thereof |
| CN101671119A (en) * | 2009-09-27 | 2010-03-17 | 上海大学 | Method for preparing Li-doped P-type zinc oxide film |
| CN101935876A (en) * | 2010-09-14 | 2011-01-05 | 浙江大学 | In-doped ZnO monodisperse nano granules and synthesizing method thereof |
| CN102936033A (en) * | 2012-12-04 | 2013-02-20 | 九江学院 | Method for preparing monodisperse zinc oxide ultrathin nanosheets |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445961A (en) * | 2008-12-15 | 2009-06-03 | 浙江大学 | Superfine Mg-doped ZnO nano wire and synthetic method thereof |
| CN101671119A (en) * | 2009-09-27 | 2010-03-17 | 上海大学 | Method for preparing Li-doped P-type zinc oxide film |
| CN101935876A (en) * | 2010-09-14 | 2011-01-05 | 浙江大学 | In-doped ZnO monodisperse nano granules and synthesizing method thereof |
| CN102936033A (en) * | 2012-12-04 | 2013-02-20 | 九江学院 | Method for preparing monodisperse zinc oxide ultrathin nanosheets |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108821327A (en) * | 2018-06-27 | 2018-11-16 | 五邑大学 | The preparation method and its application of the pineal ZnO nano microballoon of one type |
| WO2023169017A1 (en) * | 2022-03-07 | 2023-09-14 | 深圳先进技术研究院 | Zinc oxide nanorod array photo-anode and preparation method therefor |
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Application publication date: 20140521 |