CN105420808B - The synthetic method of the ZnO nano crystalline substance of In, Ga codope - Google Patents
The synthetic method of the ZnO nano crystalline substance of In, Ga codope Download PDFInfo
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- CN105420808B CN105420808B CN201510751870.7A CN201510751870A CN105420808B CN 105420808 B CN105420808 B CN 105420808B CN 201510751870 A CN201510751870 A CN 201510751870A CN 105420808 B CN105420808 B CN 105420808B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
Abstract
The present invention provides a kind of synthetic method of the ZnO nano crystalline substance of In, Ga codope, includes the following steps：Aliphatic acid indium, gallium salt, fatty acid zinc and organic solvent are mixed and are placed in reactor, magnetic agitation is uniform, is warming up to the water vapour and oxygen for vacuumizing and being removed in reaction system after 80 150 DEG C, 200 350 DEG C are then heated under inert protective atmosphere；The alcohol that temperature is 100 200 DEG C is rapidly injected in reactor, 30 120 minutes is kept the temperature, is cooled to room temperature；Reaction mixture is centrifuged, the ZnO nano for obtaining In, Ga codope is brilliant.The method of the present invention preparation process is simple, cost is relatively low, it is reproducible, be easy to industrialized production, a diameter of 5~15nm of the ZnO nano crystalline substance of In, Ga codope of acquisition, good dispersion, controllability be strong, uniform doping.
Description
Technical field
The present invention relates to technical field of nano material more particularly to a kind of synthesis sides of the ZnO nano crystalline substance of In, Ga codope
Method.
Background technology
ZnO (zinc oxide) is a kind of II-VI group compound semiconductor materials, and energy gap is 3.37eV, exciton at room temperature
Binding energy is 60meV, is semiconductor laser, ultraviolet detector, blue violet light light-emitting diodes under the mild higher temperature of preparation room
Manage the ideal material of (LED) etc..ZnO monodimension nanometer materials are had by quantum confined effect, skin effect, piezoelectric effect etc.
Optics, electricity and the piezoelectric property etc. better than body material so that it is had become the hot spot of current photoelectric information research field.
In ZnO nano crystalline substance carry out In (indium) and Ga (gallium) codope, can under the premise of keeping wurtzite structure,
It realizes adjusting of its energy band between 3.3-3.7eV, while showing apparent surface plasmon absorption effect again,
Preparing the fields such as short wavelength's nano luminescent device and nano photoelectronic devices has good application value and research significance.
The method of the ZnO nano crystalline substance of synthesis codope In and Ga is more at present, is broadly divided into physical method and chemical method
Two major classes, the former includes mainly pulsed laser deposition, magnetron sputtering method, thermal evaporation etc., and the latter includes mainly that metal is organic
Chemical vapour deposition technique, sol-gal process, hydro-thermal (solvent heat) method etc..However, above-mentioned preparation method has the disadvantage that：Equipment
Costliness, complex process, bad dispersibility, poor controllability, doping are unequal, the ZnO for In, Ga codope that especially prepared by Physical
Nanocrystalline material can not be applied in the photoelectric devices such as the solar cell of cryogenic fluid technique and light emitting diode, therefore serious limit
Its application range is made.
Invention content
The object of the present invention is to provide a kind of ZnO of In, Ga codope of low cost, controllability is good, crystalline quality is high
Nanocrystalline and its synthetic method.
A kind of synthetic method of the ZnO nano crystalline substance of In, Ga codope, includes the following steps：By aliphatic acid indium, gallium salt, fat
Fat acid zinc and organic solvent mixing are placed in reactor, and magnetic agitation is uniform, is vacuumized except dereaction after being warming up to 80-150 DEG C
Then water vapour in system and oxygen are heated to 200-350 DEG C under inert protective atmosphere；It it is 100-200 DEG C by temperature
Alcohol is rapidly injected in reactor, is kept the temperature 30-120 minutes, is cooled to room temperature；Reaction mixture is centrifuged, In, Ga are obtained
The ZnO nano of codope is brilliant.
Further, the aliphatic acid indium is stearic acid indium, myristic acid indium, tetradecylic acid indium, isooctyl acid indium, lauric acid
At least one of indium, indium acetate, caproic acid indium, sad indium, gluconic acid indium, palmitic acid indium and citric acid indium.
Further, the gallium salt is gallium nitrate, tetradecylic acid gallium, pentadecanoic acid gallium, hexadecylic acid gallium, heptadecanoic acid gallium, stearic acid
At least one of gallium or isooctyl acid gallium.
Further, the fatty acid zinc be zinc stearate, Zinc tetradecanoate, zinc Isoocatanoate, zinc laurate, zinc acetate,
In zinc propionate, zinc undecylenate, zinc gluconate, Zinc Heptylate, zinc citrate, zinc palmitate, zinc oleate or zinc linoleate extremely
Few one kind.
Further, the sum of molal quantity of the aliphatic acid indium and the gallium salt is less than or equal to mole of the fatty acid zinc
Several 20%.
Further, the organic solvent is at least one in 1- icosa alkenes, octadecyl vinyl ether or diphenyl ether
Kind.
Further, the alcohol is at least one of pentadecanol, hexadecanol, heptadecanol, octadecyl alcolol or oleyl alcohol.
Further, the inert protective atmosphere is at least one of argon gas, helium or nitrogen.
Further, the purity of the inert protective atmosphere is 99% or more.
Further, it is 3000-6000rpm/min to take the centrifugal speed of centrifugation to the reaction mixture.
The advantageous effect that the technical solution of the embodiment of the present invention is brought is：By adjusting the heating temperature of reaction solution and anti-
The size that ZnO nano crystalline substance of In, Ga codope can be controlled between seasonable is rubbed by adjusting aliphatic acid indium, gallium salt, fatty acid zinc
Practical doping content of that than that can change In and Ga in ZnO nano crystalline substance, preparation process of the present invention is simple, cost is relatively low, repeats
Property is good, is easy to industrialized production, a diameter of 5~15nm of the ZnO nano crystalline substance of In, Ga codope of acquisition, good dispersion, can
Control property is strong, uniform doping.
Description of the drawings
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, other are can also be obtained according to these attached drawings
Attached drawing.
Fig. 1 is the XRD diagram of the ZnO nano crystalline substance of In, Ga codope in embodiment 1；
Fig. 2 is the TEM photos of the ZnO nano crystalline substance of In, Ga codope in embodiment 1；
Fig. 3 is the EDS figures of the ZnO nano crystalline substance of In, Ga codope in embodiment 1；
Fig. 4 is the UV-visible-near infrared absorption figure of the ZnO nano crystalline substance of In, Ga codope in embodiment 1.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to the embodiment of the present invention
It is described in further detail.
The synthetic method of the ZnO nano crystalline substance of In, Ga codope includes the following steps：
First, aliphatic acid indium, gallium salt, fatty acid zinc and organic solvent being mixed and is placed in reactor, magnetic agitation is uniform,
It is warming up to the water vapour and oxygen for vacuumizing and being removed in reaction system after 80-150 DEG C, is then heated under inert protective atmosphere
200-350℃；
Secondly, the alcohol that temperature is 100-200 DEG C is rapidly injected in reactor, keeps the temperature 30-120 minutes, is cooled to room
Temperature；
Finally, reaction mixture is centrifuged, the ZnO nano for obtaining In, Ga codope is brilliant.
Aliphatic acid indium can be stearic acid indium, myristic acid indium, tetradecylic acid indium, isooctyl acid indium, lauric acid indium, indium acetate,
At least one of caproic acid indium, sad indium, gluconic acid indium, lauric acid indium, palmitic acid indium or citric acid indium.
Gallium salt can be gallium nitrate, tetradecylic acid gallium, pentadecanoic acid gallium, hexadecylic acid gallium, heptadecanoic acid gallium, stearic acid gallium, isooctyl acid
At least one of gallium.
Fatty acid zinc can be zinc stearate, Zinc tetradecanoate, zinc Isoocatanoate, zinc laurate, zinc acetate, zinc propionate, ten
At least one of monoenoic acid zinc, zinc gluconate, Zinc Heptylate, zinc citrate, zinc palmitate, zinc oleate or zinc linoleate.
The sum of molal quantity of aliphatic acid indium and gallium salt is less than or equal to the 20% of the molal quantity of fatty acid zinc.
Organic solvent can be at least one of 1- icosa alkenes, octadecyl vinyl ether or diphenyl ether.
Alcohol can be at least one of pentadecanol, hexadecanol, heptadecanol, octadecyl alcolol or oleyl alcohol.
Inert protective atmosphere is at least one of argon gas, helium or the nitrogen that purity is 99% or more.
It is 3000-6000rpm/min to take the centrifugal speed of centrifugation to reaction mixture.
Reactor can be flask, beaker or other glass containers.
Embodiment 1
First, weighing 0.1mmol lauric acid indium, 0.05mmol tetradecylic acids gallium, 1mmol zinc stearates, (i.e. molar ratio is 10：
5: 100) it with 15ml octadecyl vinyl ether is placed in 50ml reaction flask, is warming up to 140 DEG C under magnetic stirring, it is then right
Reaction flask vacuumizes 25 minutes, to remove the water vapour and oxygen in reaction system, in the protection that purity is 99.99% helium
Reaction solution is brought rapidly up to 300 DEG C under atmosphere；
Secondly, the octadecyl alcolol that temperature is 180 DEG C is injected into reaction flask rapidly, and keeps the temperature 40 minutes, it is cold with water-bath
But reaction solution is to room temperature；
Finally, reaction mixture 6000rpm/min is centrifuged, the ZnO nano for obtaining In, Ga codope is brilliant.
After the ZnO nano crystalline substance product drying of In, Ga codope of obtained white, carries out XRD (X-ray diffraction) and survey
Examination, TEM Electronic Speculum are taken pictures, EDS tests and UV-visible-near infrared absorption figure measure.
Fig. 1 is the XRD diagram of the ZnO nano crystalline substance of In, Ga codope in embodiment 1, shown in Figure 1, in XRD test results
Peak be all buergerite ZnO phases main peak position, In, Ga introduce after, the ZnO nano crystalline substance of In, Ga codope still remains
The original buergerite phase structures of ZnO, that is, the product proved are wurtzite structure.
Fig. 2 is the TEM photos of the ZnO nano crystalline substance of In, Ga codope in embodiment 1, shown in Figure 2, can in TEM photos
To find out, a diameter of 7~10nm of the ZnO nano crystalline substance of In, Ga codope, the dispersion of the ZnO nano crystalline substance of In, Ga codope is equal
It is even, favorable dispersibility.
Fig. 3 is the EDS figures of the ZnO nano crystalline substance of In, Ga codope in embodiment 1, shown in Figure 3, it is known that the master of product
It is tetra- kinds of elements of In, Ga, Zn, O to want ingredient, it was demonstrated that In, Ga element are adulterated really into ZnO nano crystalline substance.
Fig. 4 is the UV-visible-near infrared absorption figure of the ZnO nano crystalline substance of In, Ga codope in embodiment 1, referring to
Shown in Fig. 4, this is nanocrystalline to have and is significantly absorbed at two, and the absorption peak at 340nm is the Intrinsic Gettering of ZnO, due to drawing for In, Ga
Enter and the variation of doping, can effectively make absorption peak position blue shift, that is, adjust nanocrystalline energy gap；At long-wave band
Absorption be surface plasmon absorption, the doping of provable In, Ga significantly improve the current-carrying of the nanocrystalline material
Sub- concentration.This is nanocrystalline to show significant visible region completely through the characteristic that infrared light district obviously absorbs illustrates that it is one
The extraordinary transparent conductive material of kind.
Embodiment 2
First, weighing 0.05mmol tetradecylic acids indium, 0.05mmol gallium nitrates, 1mmol zinc Isoocatanoates, (i.e. molar ratio is 5：5∶
100) it is placed in 50ml reaction flasks with 15ml1- icosa alkenes, is warming up to 150 DEG C under magnetic stirring, then reaction flask is taken out
Vacuum 30 minutes will be anti-in the case where purity is the protective atmosphere of 99.99% helium to remove the water vapour and oxygen in reaction system
Solution is answered to be brought rapidly up to 260 DEG C；
Secondly, the pentadecanol that temperature is 200 DEG C is injected into reaction flask rapidly, and keeps the temperature 70 minutes, it is cold with water-bath
But reaction solution is to room temperature；
Finally, reaction mixture 4000rpm/min is centrifuged, the ZnO nano for obtaining In, Ga codope is brilliant.
After measured, 7~11nm of diameter of the ZnO nano crystalline substance of In, Ga codope obtained.
Embodiment 3
First, weigh that 0.01mmol myristic acids indium, 0.05mmol isooctyl acids gallium, (i.e. molar ratio is 1mmol zinc laurates
1：5: 100) being placed in 50ml reaction flasks with 15ml diphenyl ether, 100 DEG C are warming up under magnetic stirring, then to reaction flask
It vacuumizes 40 minutes, it, will in the case where purity is the protective atmosphere of 99.99% helium to remove the water vapour and oxygen in reaction system
Reaction solution is brought rapidly up to 310 DEG C；
Secondly, the oleyl alcohol that temperature is 190 DEG C is injected into reaction flask rapidly, and keeps the temperature 50 minutes, use water-bath cooling
Reaction solution is to room temperature；
Finally, reaction mixture 5000rpm/min is centrifuged, the ZnO nano for obtaining In, Ga codope is brilliant.
After measured, 8~12nm of diameter of the ZnO nano crystalline substance of In, Ga codope obtained.
Embodiment 4
First, weigh that 0.1mmol stearic acid indium, 0.1mmol heptadecanoic acids gallium, (i.e. molar ratio is 1mmol Zinc tetradecanoates
10：10: 100) being placed in 50ml reaction flasks with 15ml diphenyl ether, be warming up to 80 DEG C under magnetic stirring, then reaction is burnt
Bottle vacuumizes 25 minutes, to remove the water vapour and oxygen in reaction system, in the case where purity is the protective atmosphere of 99.99% helium
Reaction solution is brought rapidly up to 350 DEG C；
Secondly, the oleyl alcohol that temperature is 190 DEG C is injected into reaction flask rapidly, and keeps the temperature 30 minutes, use water-bath cooling
Reaction solution is to room temperature；
Finally, reaction mixture 3000rpm/min is centrifuged, the ZnO nano for obtaining In, Ga codope is brilliant.
After measured, 5~8nm of diameter of the ZnO nano crystalline substance of In, Ga codope obtained.
Embodiment 5
First, weighing 0.01mmol isooctyl acids indium, 0.01mmol pentadecanoic acids gallium, 1mmol indium acetates, (i.e. molar ratio is 1：1：
100) it is placed in 50ml reaction flasks with 15ml diphenyl ether, is warming up to 150 DEG C under magnetic stirring, then reaction flask taken out true
It is 35 minutes empty, it, will reaction in the case where purity is the protective atmosphere of 99.99% helium to remove the water vapour and oxygen in reaction system
Solution is brought rapidly up to 200 DEG C；
Secondly, the oleyl alcohol that temperature is 100 DEG C is injected into reaction flask rapidly, and keeps the temperature 120 minutes, use water-bath cooling
Reaction solution is to room temperature；
Finally, reaction mixture 4500rpm/min is centrifuged, the ZnO nano for obtaining In, Ga codope is brilliant.
After measured, 10~15nm of diameter of the ZnO nano crystalline substance of In, Ga codope obtained.
It is found that In, Ga can be controlled by the heating temperature and reaction time for adjusting reaction solution from above-described embodiment
The size of the ZnO nano crystalline substance of codope.It is constant to control other reaction conditions, reaction time length extends, and crystal growth increases, reaction
Time shortens, and crystal growth reduces.It can change ZnO nano crystalline substance by the molar ratio of adjusting aliphatic acid indium, gallium salt, fatty acid zinc
The practical doping content of middle In and Ga realizes that the band gap at room temperature of ZnO nano crystalline substance is adjusted in certain electron-volt range.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of synthetic method of the ZnO nano crystalline substance of In, Ga codope, which is characterized in that include the following steps：
Aliphatic acid indium, gallium salt, fatty acid zinc and organic solvent are mixed and are placed in reactor, magnetic agitation is uniform, is warming up to 80-
The water vapour and oxygen removed in reaction system is vacuumized after 150 DEG C, is then heated to 200-350 under inert protective atmosphere
DEG C, the sum of molal quantity of the aliphatic acid indium and the gallium salt is less than or equal to the 20% of the molal quantity of the fatty acid zinc；
The alcohol that temperature is 100-200 DEG C is rapidly injected in reactor, 30-120 minutes is kept the temperature, is cooled to room temperature；
Reaction mixture is centrifuged, the ZnO nano for obtaining In, Ga codope is brilliant.
2. the synthetic method of the ZnO nano crystalline substance of In, Ga codope as described in claim 1, which is characterized in that the aliphatic acid
Indium is stearic acid indium, myristic acid indium, isooctyl acid indium, lauric acid indium, indium acetate, caproic acid indium, sad indium, gluconic acid indium, palm fibre
At least one of palmitic acid acid indium and citric acid indium.
3. the synthetic method of the ZnO nano crystalline substance of In, Ga codope as described in claim 1, which is characterized in that the gallium salt is
At least one of gallium nitrate, tetradecylic acid gallium, pentadecanoic acid gallium, hexadecylic acid gallium, heptadecanoic acid gallium, stearic acid gallium or isooctyl acid gallium.
4. the synthetic method of the ZnO nano crystalline substance of In, Ga codope as described in claim 1, which is characterized in that the aliphatic acid
Zinc is zinc stearate, Zinc tetradecanoate, zinc Isoocatanoate, zinc laurate, zinc acetate, zinc propionate, zinc undecylenate, gluconic acid
At least one of zinc, Zinc Heptylate, zinc citrate, zinc palmitate, zinc oleate or zinc linoleate.
5. the synthetic method of the ZnO nano crystalline substance of In, Ga codope as described in claim 1, which is characterized in that described organic molten
Agent is at least one of 1- icosa alkenes, octadecyl vinyl ether or diphenyl ether.
6. the synthetic method of the ZnO nano crystalline substance of In, Ga codope as described in claim 1, which is characterized in that the alcohol is ten
At least one of pentol, hexadecanol, heptadecanol, octadecyl alcolol or oleyl alcohol.
7. the synthetic method of the ZnO nano crystalline substance of In, Ga codope as described in claim 1, which is characterized in that the inertia is protected
It is at least one of argon gas, helium or nitrogen to protect atmosphere.
8. the synthetic method of the ZnO nano crystalline substance of In, Ga codope as described in claim 1, which is characterized in that the inertia is protected
The purity for protecting atmosphere is 99% or more.
9. the synthetic method of the ZnO nano crystalline substance of In, Ga codope as described in claim 1, which is characterized in that the reaction
It is 3000-6000rpm/min that mixture, which takes the centrifugal speed of centrifugation,.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101582304A (en) * | 2008-05-13 | 2009-11-18 | 日东电工株式会社 | Transparent conductive film and method for production thereof |
| CN201754405U (en) * | 2010-07-16 | 2011-03-02 | 北京工业大学 | Zinc-oxide doped PN homojunction |
| CN103130493A (en) * | 2011-11-23 | 2013-06-05 | 财团法人工业技术研究院 | Indium Gallium Zinc Oxide (IGZO) nano powder and preparation method and application thereof |
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| CN101445961B (en) * | 2008-12-15 | 2011-06-15 | 浙江大学 | Superfine Mg-doped ZnO nano wire and synthetic method thereof |
| CN101872663A (en) * | 2010-06-18 | 2010-10-27 | 上海交通大学 | Preparation method of gallium-doped zinc oxide nano-particle |
| CN101935876A (en) * | 2010-09-14 | 2011-01-05 | 浙江大学 | In-doped ZnO monodisperse nano granules and synthesizing method thereof |
| CN101935875B (en) * | 2010-09-14 | 2012-02-15 | 浙江大学 | Sn-doped ZnO superfine nanowires and synthesis method thereof |
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| CN101582304A (en) * | 2008-05-13 | 2009-11-18 | 日东电工株式会社 | Transparent conductive film and method for production thereof |
| CN201754405U (en) * | 2010-07-16 | 2011-03-02 | 北京工业大学 | Zinc-oxide doped PN homojunction |
| CN103130493A (en) * | 2011-11-23 | 2013-06-05 | 财团法人工业技术研究院 | Indium Gallium Zinc Oxide (IGZO) nano powder and preparation method and application thereof |
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